CN106995402B - Equipment for producing fine-carbody and process for producing fine-carbody by utilizing static melting crystallization method - Google Patents
Equipment for producing fine-carbody and process for producing fine-carbody by utilizing static melting crystallization method Download PDFInfo
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- CN106995402B CN106995402B CN201710068740.2A CN201710068740A CN106995402B CN 106995402 B CN106995402 B CN 106995402B CN 201710068740 A CN201710068740 A CN 201710068740A CN 106995402 B CN106995402 B CN 106995402B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D209/56—Ring systems containing three or more rings
- C07D209/80—[b, c]- or [b, d]-condensed
- C07D209/82—Carbazoles; Hydrogenated carbazoles
- C07D209/84—Separation, e.g. from tar; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D209/56—Ring systems containing three or more rings
- C07D209/80—[b, c]- or [b, d]-condensed
- C07D209/82—Carbazoles; Hydrogenated carbazoles
- C07D209/86—Carbazoles; Hydrogenated carbazoles with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached to carbon atoms of the ring system
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention relates to a device for producing refined carbolic acid, which comprises a crude anthracene dissolving and melting system, a solvent crystallization system, a solvent oil recovery and regeneration system, a carbolic acid separating system and a static melting system. Also provides a process for producing high-purity refined naphthalene by using the device for producing refined kaka. The invention has the beneficial effects that: compared with the prior art, the static melting crystallization method of the invention uses crude anthracene as the main raw material to produce the fine-carbolic acid, and has the characteristics of less process links, less use equipment, low production cost, low labor intensity of workers, less energy consumption, no environmental pollution and the like; the production efficiency is effectively improved, and the production operation environment of workers is improved.
Description
Technical Field
The invention relates to the field of tar deep processing, in particular to a tar deep processing distillation and crystallization process comprising raw material pretreatment and static melting crystallization.
Background
At present, no process really realizes environment protection, energy saving and safe and automatic operation in various production processes of fine kaka at home and abroad. The production of fine carbo is generally accomplished by multiple solvent washes of crude anthracene or anthracene oil. The production process has the advantages of multiple process links, more needed devices, high production cost, incapability of realizing automatic control, high labor intensity of workers, more energy consumption, great environmental pollution and great reduction of production efficiency.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: provides a device for producing fine carbody and a process for producing fine carbody by using a static melting crystallization method.
The invention adopts the technical proposal for solving the problems that:
an apparatus for producing refined carboline comprises a crude anthracene dissolving and melting system, a solvent crystallization system, a solvent oil recovery and regeneration system, a carboline separation system and a static melting system.
The crude anthracene dissolving and melting system comprises a melting tank 1, a melting crude anthracene delivery pump a2, a melting crude anthracene buffer tank 3, a melting crude anthracene delivery pump b4, a crude anthracene solvent proportioning tank 6 and a post-preparation delivery pump 7, wherein the melting tank 1 is communicated with the melting crude anthracene buffer tank 3 through a pipeline, the melting crude anthracene delivery pump a2 is arranged on the pipeline, the melting crude anthracene buffer tank 3 is communicated with the crude anthracene solvent proportioning tank 6 through a pipeline, the melting crude anthracene delivery pump b4 is arranged on the pipeline, the post-preparation delivery pump 7 is connected with a solvent crystallizer 5 through the pipeline, and the post-preparation delivery pump 7 is arranged on the pipeline.
The solvent crystallization system comprises a solvent crystallizer 5, a solvent crystallization heat conduction oil delivery pump 8, a primary cooler 9, a deep cooler 10, a heater 11, a mother liquor buffer tank 12, a solvent crystallization mother liquor delivery pump 13, a solvent crystallization product tank 23 and a solvent crystallization product pump 24, wherein the primary cooler 9, the deep cooler 10 and the heater 11 are respectively communicated with the solvent crystallizer 5 through pipelines, the solvent crystallization heat conduction oil delivery pump 8 is arranged on the pipelines, the solvent crystallizer 5 is connected with the mother liquor buffer tank 12 and the solvent crystallization product tank 23, the mother liquor buffer tank 12 is connected with the solvent regeneration tower 14 through the pipelines, the solvent crystallization mother liquor delivery pump 13 is arranged on the pipelines, the solvent crystallization product tank 23 is connected with the concentration tower 25 through the pipelines, and the solvent crystallization product pump 24 is arranged on the pipelines.
The solvent oil recovery regeneration system comprises a solvent regeneration tower 14, a phenanthrene residual oil delivery pump 15, a regeneration tower top condenser 16, a regeneration tower bottom reboiler 17, a heat conduction oil heating furnace a18, a solvent oil storage tank 19, a solvent oil delivery pump 20 and a heat conduction oil delivery pump a21, wherein the top of the solvent regeneration tower 14 is provided with the regeneration tower top condenser 16, the upper part of the solvent regeneration tower 14 is communicated with the solvent oil storage tank 19, a pipeline of the solvent oil storage tank 19 is connected with a melting tank 1 and a crude anthracene solvent proportioning tank 6, the pipeline is provided with the solvent oil delivery pump 20, the bottom of the solvent regeneration tower 14 is connected with the phenanthrene residual oil delivery pump 15, the solvent regeneration tower 14 is connected with the regeneration tower bottom reboiler 17 in parallel, the regeneration tower bottom reboiler 17 is connected with the heat conduction oil heating furnace a18 through the pipeline, and the pipeline is provided with the heat conduction oil delivery pump a21.
The carboline separating system comprises a concentrating tower 25, a concentrating tower top condenser 26, a concentrating tower bottom reboiler 27, a heat conducting oil circulating pump b28, a heat conducting oil heating furnace b29, a carboline conveying pump 30, a carboline distilling tower 31, a reflux tank 32, a reflux pump 33, a carboline extracting pump 34, a carboline extracting pump 35, a carboline distilling tower bottom reboiler 36, a carboline buffer tank 37 and a carboline conveying pump 38, wherein the concentrating tower top is provided with the concentrating tower top condenser 26, the concentrating tower 25 bottom is provided with the concentrating tower bottom reboiler 27, the concentrating tower 25 is connected with the carboline distilling tower 31 through a pipeline, the pipeline between the carboline distilling tower 31 and the reflux tank 32 is provided with the reflux pump 33, the carboline extracting pump 34 is arranged at the carboline extracting outlet of the carboline distilling tower 31, the carboline distilling tower bottom is provided with the carboline extracting pump 36, the carboline extracting tank 37 is connected with the carboline extracting tower bottom reboiler 31 through a pipeline, the pipeline between the carboline distilling tower 31 and the carboline reboiler 37 is provided with the carboline extracting tower bottom reboiler 35, the heat conducting oil circulating pump is connected with the carboline conveying tower bottom reboiler 37 through the pipeline after the carboline rectifying tower bottom reboiler 27, and the heat conducting oil circulating pump is connected with the crude heat conducting oil circulating pump 37.
The static melting system comprises a static melting crystallizer 39, a refined carbazole tank 40, a refined carbazole delivery pump 41, a molten crystallization residual liquid tank 42, a molten crystallization residual liquid delivery pump 43, a flaker 44, a bin 45, a molten crystallization heat-conducting oil circulating pump 46, an air cooler 47 and a molten crystallization heater 48, wherein the air cooler 47 and the molten crystallization heater 48 are respectively communicated with the static melting crystallizer 39 through pipelines, the pipeline is provided with the molten crystallization heat-conducting oil circulating pump 46, the refined carbazole tank 40 and the molten crystallization residual liquid tank 42 are connected behind the static melting crystallizer 39, the refined carbazole delivery pump 41 is arranged in the refined carbazole tank 40, the molten crystallization residual liquid delivery pump 43 is arranged in the molten crystallization residual liquid tank 42, the refined carbazole delivery pump 41 and the molten crystallization residual liquid delivery pump 43 are connected behind the flaker 44, and the bin 45 is connected behind the flaker 44.
The heating mode of the solvent regeneration tower 14 in the solvent oil recovery and regeneration operation is a thermosiphon indirect heating mode, the heat conduction oil circularly flows between a heat conduction oil heating furnace a18 and a shell side of a reboiler 17 at the bottom of the regeneration tower through a heat conduction oil circulating pump 28b, the material at the bottom of the solvent regeneration tower 14 circularly flows between the bottom of the tower and the shell side or the tube side of the thermosiphon reboiler by utilizing density difference, and heat generated by gas combustion of the heat conduction oil heating furnace a18 is transferred to the material at the bottom of the regeneration tower through the thermosiphon reboiler.
The static melting crystallizer 39 of the main equipment for static melting crystallization operation is of a finned tube structure in a box body, a feed inlet and a discharge outlet are arranged at the bottom of the box body, the static melting crystallizer 39 is of a static melting crystallizer 39 with a breathing tube orifice at the top, the box body can be a cylinder or a tetragonal body, a jacket is arranged outside the box body, and three thermometers with different installation positions are arranged in the box body; the quality of the refined carbazole product can be effectively adjusted by adjusting the temperature at the end of crystallization cooling so as to meet different customer demands.
A process for producing high-purity refined naphthalene by using a device for producing refined kaka comprises the following steps:
adding solvent oil into crude anthracene to melt in a crude anthracene melting tank 1, caching the melted crude anthracene and solvent oil by a crude anthracene melting tank 3, and then sending the crude anthracene and solvent oil into a solvent crystallizer 5, and cooling the crude anthracene and the solvent oil by a primary cooler 9 and a deep cooler 10 in two steps until the temperature is reduced to 8 ℃; in the cooling process, the carboline and the anthracene are gradually crystallized and separated out, and phenanthrene and other impurities in the crude anthracene are discharged as mother liquor after crystallization together with solvent oil; mother liquor discharged from the solvent crystallizer 5 is sent to a solvent regeneration tower 14 after being buffered by a mother liquor buffer tank 12, solvent oil is recovered to a solvent oil storage tank 19 through distillation operation, and is sent to a melting tank 1 and a crude anthracene solvent proportioning tank 6 for repeated use, and the regeneration tower residual liquid after solvent oil removal is used as a product to be sold to carbon black production or tar hydrogenation manufacturers; after the mother solution is discharged, fresh solvent oil is added into the solvent crystallizer 5 for a plurality of times, and recrystallization is carried out for a plurality of times, and each recrystallization is also subjected to the processes of adding the solvent oil, primary cooling, deep cooling and mother solution discharge; after the completion of the multiple crystallization, the solvent oil is filled into the solvent crystallizer 5, the heater 11 is used for heating to 120 ℃ to completely dissolve the crystal, the mixture of the dissolved carboline and the solvent oil is sent to the concentration tower 25 and the anthracene carboline distillation tower 31, the solvent oil is distilled and extracted in the concentration tower 25 for recycling, the concentrated anthracene carboline is sent to the anthracene carboline distillation tower 31, and the carboline is separated from the anthracene through reduced pressure distillation to obtain crude carbazole with the purity of about 92%; finally, the crude carbazole is sent to a static melting crystallizer 39, and refined carboline with purity more than 98% is produced through static melting crystallization; the whole process except for transporting crude anthracene is automatically operated and completed in a DCS distributed control system.
The heating mode of the solvent regeneration tower 14 in the solvent oil recovery and regeneration operation is a thermosiphon indirect heating mode, the heat conduction oil circularly flows between a heat conduction oil heating furnace 18a and a shell side or a tube side of a reboiler 17 at the bottom of the regeneration tower through a heat conduction oil circulating pump 28b, the material at the bottom of the solvent regeneration tower 14 circularly flows between the bottom of the tower and the shell side or the tube side of the thermosiphon reboiler by utilizing density difference, and heat generated by gas combustion of the heat conduction oil heating furnace 18a is transferred to the material at the bottom of the regeneration tower through the thermosiphon reboiler.
The static melting crystallizer 39 of the main equipment for static melting crystallization operation is of a finned tube structure in a box body, a feed inlet and a discharge outlet are arranged at the bottom of the box body, the static melting crystallizer 39 is of a static melting crystallizer 39 with a breathing tube orifice at the top, the box body can be a cylinder or a tetragonal body, a jacket is arranged outside the box body, and three thermometers with different installation positions are arranged in the box body; the quality of the refined carbazole product can be effectively adjusted by adjusting the temperature at the end of crystallization cooling so as to meet different customer demands.
The invention has the beneficial effects that: the pretreatment of the crude anthracene for solvent crystallization is a multi-stage crystallization process, the first-stage crystallization process is to add a mixed solution of the melted crude anthracene and the solvent oil into a solvent crystallizer, and the other crystallization processes are to add the solvent oil into the solvent crystallizer, so that the quality of the carboanthracene crystal after solvent crystallization can be adjusted by adjusting the crystallization stage number, and the quality of the final refined carbazole product can be further adjusted. Compared with the prior art, the static melting crystallization method of the invention uses crude anthracene as the main raw material to produce the fine-carbolic acid, and has the characteristics of less process links, less use equipment, low production cost, low labor intensity of workers, less energy consumption, no environmental pollution and the like; the production efficiency is effectively improved, and the production operation environment of workers is improved.
Drawings
Fig. 1 is a diagram showing the configuration of a process apparatus for producing fine carbolines by using crude anthracene as a main raw material in a static melt crystallization method.
The process comprises the steps of 1-melting tank, 2-melting crude anthracene delivery pump a, 3-melting crude anthracene buffer tank, 4-melting crude anthracene delivery pump b, 5-solvent crystallizer, 6-crude anthracene solvent proportioning tank, 7-matched delivery pump, 8-solvent crystallization heat conduction oil delivery pump, 9-primary cooler, 10-deep cooler, 11-heater, 12-mother liquor buffer tank, 13-solvent crystallization mother liquor delivery pump, 14-solvent regeneration tower, 15-phenanthrene residual oil delivery pump, 16-regeneration tower top condenser, 17-regeneration tower bottom reboiler, 18-heat conduction oil heating furnace a, 19-solvent oil storage tank, 20-solvent oil delivery pump, 21-heat conduction oil delivery pump a, 23-solvent crystallization product tank, 24-solvent crystallization product pump, 25-concentration tower, 26-concentration tower top condenser, 27-concentration tower bottom reboiler, 28-heat conduction oil circulation pump b, 29-heat conduction oil heating furnace b, 30-carboanthracene oil delivery pump, 31-anthracene carboline distillation tower, 32-reflux tank, 33-reflux pump, 34-carboline reboiler, 35-carboline pump, 35-solvent oil storage tank, 20-solvent oil delivery pump, 25-concentration tower top condenser, 27-concentration tower bottom condenser, 27-heat conduction oil circulation pump, 35-34-carboline crystallization tower bottom pump, 35-40-vacuum pump, 43-concentration tower bottom tank, 43-vacuum pump, 43-circulation pump, 43-vacuum pump, 43-type crude crystal tower bottom tank, 43-vacuum pump, 43-circulation pump, and 43-tank, and the like.
Detailed Description
Embodiments of the present invention are further described below with reference to the accompanying drawings.
Example 1:
the equipment used in the process for producing the fine carboline by taking crude anthracene as a main raw material in the static melting crystallization method comprises a crystallizer, a distillation tower, a chemical pump, a storage tank and the like, and the specific description is shown in the accompanying drawings; the device connection relationship and the process flow are the same as those shown in the drawings and described above for the industrial flow.
The process comprises the following steps: adding crude anthracene and solvent oil into a melting tank 1 together, conveying the crude anthracene and the solvent oil to a melting crude anthracene buffer tank 3 by a melting crude anthracene conveying pump a2 after melting, simultaneously conveying the melted crude anthracene and the solvent oil to a crude anthracene solvent proportioning tank 6 according to the proportion of 1:3, conveying the crude anthracene and the solvent oil to a solvent crystallizer 5 by a proportioning rear conveying pump 7, and operating four-level crystallization in the solvent crystallizer; discharging the mother liquor of the first-stage operation to a solvent crystallization mother liquor buffer tank 12, and conveying the mother liquor to a solvent regeneration tower 14 for regeneration by a solvent crystallization mother liquor conveying pump 13; the product after the fourth-stage operation is discharged to a solvent crystallization product tank 23, and is conveyed to a concentration tower 25 by a solvent crystallization product pump 24, and the concentrated carbofuran oil is conveyed to an anthracene carbofuran distillation tower 31 by a carbofuran oil conveying pump 30; 91.0% of crude carbazole is extracted to a crude carbazole buffer tank 37 through a crude carbazole extraction pump 35, the crude carbazole is sent to a melting crystallizer 39 through a crude carbazole delivery pump 38, the crude carbazole starts to be slowly cooled at about 242 ℃ until 225 ℃, then residual liquid is discharged to a melting crystallization residual liquid tank 42, the residual liquid is sent to a flaker 44 by a melting crystallization residual liquid pump 43 for flaking, crystals in the melting crystallizer 39 are indirectly heated to 250 ℃ through a melting crystallization heater, and then are discharged to a refined carbazole tank 40, so that a refined carbazole product with the mass of 98.1% is obtained, and refined carbazole is sent to the flaker 44 for flaking through a refined carbazole delivery pump 41; and (5) sheeting the refined carbazole and the residual liquid in different time periods by using a sheeting machine, and respectively packaging and selling.
Example 2:
the static melt crystallization method uses the same equipment as in example 1 as the process for producing fine carbolic acid from crude anthracene as the main raw material.
The process comprises the following steps: adding crude anthracene and solvent oil into a melting tank 1 together, conveying the crude anthracene and the solvent oil to a melting crude anthracene buffer tank 3 by a melting crude anthracene conveying pump a2 after melting, simultaneously conveying the melted crude anthracene and the solvent oil to a crude anthracene solvent proportioning tank 6 according to the proportion of 1:3, conveying the crude anthracene and the solvent oil to a solvent crystallizer 5 by a proportioning rear conveying pump 7, and operating five-level crystallization in the solvent crystallizer; discharging the mother liquor of the first-stage operation to a solvent crystallization mother liquor buffer tank 12, and conveying the mother liquor to a solvent regeneration tower 14 for regeneration by a solvent crystallization mother liquor conveying pump 13; the product after the fifth-stage operation is discharged to a solvent crystallization product tank 23, and is conveyed to a concentration tower 25 by a solvent crystallization product pump 24, and the concentrated carbofuran oil is conveyed to an anthracene carbofuran distillation tower 31 by a carbofuran oil conveying pump 30; 92.5% of crude carbazole is extracted to a crude carbazole buffer tank 37 through a crude carbazole extraction pump 35, the crude carbazole is sent to a melting crystallizer 39 through a crude carbazole delivery pump 38, the crude carbazole starts to be slowly cooled at about 242 ℃ until the crude carbazole reaches 228 ℃, then the residual liquid is discharged to a melting crystallization residual liquid tank 42, the residual liquid is sent to a flaker 44 by a melting crystallization residual liquid pump 43, crystals in the melting crystallizer 39 are indirectly heated to 250 ℃ through a melting crystallization heater, and then the crystals are discharged to a refined carbazole tank 40, so that a refined carbazole product with the mass of 98.9% is obtained, and the refined carbazole is sent to the flaker 44 by a refined carbazole delivery pump 41 for flaking; and (5) sheeting the refined carbazole and the residual liquid in different time periods by using a sheeting machine, and respectively packaging and selling.
The embodiments of the present invention are not limited to the above embodiments, and all the similar structures and variations using the present invention are within the scope of the present invention.
Claims (4)
1. An apparatus for producing a fine click, characterized in that: the system comprises a crude anthracene dissolving and melting system, a solvent crystallization system, a solvent oil recovery and regeneration system, a carboanthracene separation system and a static melting system, wherein the crude anthracene dissolving and melting system comprises a melting tank (1), a melting crude anthracene conveying pump a (2), a melting crude anthracene buffer tank (3), a melting crude anthracene conveying pump b (4), a crude anthracene solvent distributing tank (6) and a matched conveying pump (7), the melting tank (1) is communicated with the melting crude anthracene buffer tank (3) through a pipeline, the melting crude anthracene conveying pump a (2) is arranged on the pipeline, the melting crude anthracene buffer tank (3) is communicated with the crude anthracene solvent distributing tank (6) through a pipeline, the melted crude anthracene conveying pump b (4) is arranged on the pipeline, the matched conveying pump (7) is connected with a solvent crystallizer (5) through a pipeline, the matched conveying pump (7) is arranged on the pipeline, the solvent crystallization system comprises a solvent crystallizer (5), a solvent crystallization heat conducting oil conveying pump (8), a primary cooler (9), a deep cooler (10), a heater (11), a mother liquor tank (12), a solvent crystallization mother liquor conveying pump (13), a solvent crystallization product (23) and a solvent crystallizer (24) are respectively communicated with the solvent crystallizer (11) through the pipeline, the heat conducting pump (9) and the solvent crystallizer (11) through the pipeline, the solvent crystallizer (5) is connected with a mother liquor buffer tank (12) and a solvent crystallization product tank (23), the mother liquor buffer tank (12) is connected with a solvent regeneration tower (14) through a pipeline, a solvent crystallization mother liquor delivery pump (13) is arranged on the pipeline, the solvent crystallization product tank (23) is connected with a concentration tower (25) through the pipeline, a solvent crystallization product pump (24) is arranged on the pipeline, the solvent oil recovery regeneration system comprises the solvent regeneration tower (14), a phenanthrene residual oil delivery pump (15), a regeneration tower top condenser (16), a regeneration tower bottom reboiler (17), a heat conducting oil heating furnace a (18), a solvent oil storage tank (19), a solvent oil delivery pump (20) and a heat conducting oil delivery pump a (21), the top of the solvent regeneration tower (14) is provided with a regeneration tower top condenser (16), the upper part of the solvent regeneration tower (14) is communicated with the solvent oil storage tank (19), the solvent oil storage tank (19) is connected with a melting tank (1) and a crude anthracene solvent distribution pump (6) through the pipeline, the bottom of the solvent regeneration tower (14) is connected with a phenanthrene residual oil delivery pump (15), the solvent regeneration tower reboiler (14) is connected with the heat conducting oil delivery pump (17) in parallel, the heat conducting oil is connected with the heat conducting oil delivery tank (21) through the heat conducting oil delivery tank (17), the anthracene separation system comprises a concentration tower (25), a concentration tower top condenser (26), a concentration tower bottom reboiler (27), a heat conduction oil circulating pump b (28), a heat conduction oil heating furnace b (29), an anthracene oil conveying pump (30), an anthracene-based distillation tower (31), a reflux tank (32), a reflux pump (33), an anthracene extraction pump (34), a crude anthracene extraction pump (35), an anthracene distillation tower bottom reboiler (36), a crude anthracene buffer tank (37) and a crude anthracene conveying pump (38), wherein the top of the concentration tower (25) is provided with a concentration tower top condenser (26), the bottom of the concentration tower (25) is provided with a concentration tower bottom reboiler (27), the concentration tower (25) is provided with an anthracene-based distillation tower (31) after passing through a pipeline, the anthracene oil conveying pump (30) is arranged on the pipeline, the top of the anthracene distillation tower (31) is connected with the reflux tank (32), the reflux pump (33) is arranged on the pipeline between the anthracene distillation tower (31), the anthracene extraction pump (34) is arranged on the anthracene outlet of the anthracene distillation tower (31), the anthracene (31) bottom of the anthracene extraction tower bottom is provided with an anthracene extraction pump (37), the anthracene tower bottom (31) is provided with an anthracene extraction pipeline (37) after the anthracene distillation tower (31) is arranged between the crude anthracene tower bottom (31), the thick carboline buffer tank (37) is connected with the static melting crystallizer (39) through a pipeline, the thick carboline conveying pump (38) is arranged in the thick carboline buffer tank (37), the concentrated tower bottom reboiler (27) and the anthracene distillation tower bottom reboiler (36) are both connected with the heat conduction oil heating furnace b (29) through pipelines, the heat conduction oil circulating pump b (28) is arranged on the pipelines, the static melting system comprises the static melting crystallizer (39), the refined carbazole tank (40), the refined carbazole conveying pump (41), the molten crystallization residual liquid tank (42), the molten crystallization residual liquid conveying pump (43), the flaker (44), the stock bin (45), the molten crystallization heat conduction oil circulating pump (46), the air cooler (47) and the molten crystallization heater (48) are respectively communicated with the static melting crystallizer (39) through pipelines, the molten crystallization heat conduction oil circulating pump (46) is arranged on the pipelines, the static melting crystallizer (39) is connected with the refined carbazole tank (40) and the molten crystallization residual liquid tank (42), the refined carbazole tank (40) is internally provided with the refined carbazole conveying pump (41), the molten crystallization residual liquid tank (42) is internally provided with the refined carbazole conveying pump (43), the molten crystallization residual liquid (43) is internally provided with the refined carbazole conveying pump (43), the molten residual liquid is conveyed by the refined carbazole pump (43), the flaker (44) is connected with a stock bin (45) in the back.
2. An apparatus for producing a fine click as defined in claim 1, wherein: the heating mode of the solvent regeneration tower (14) in the solvent oil recovery and regeneration operation is a thermosiphon indirect heating mode, the heat conduction oil circularly flows between a heat conduction oil heating furnace a (18) and a tube side or a shell side of a regeneration tower bottom reboiler (17) through a heat conduction oil circulating pump b (28), the tower bottom material of the solvent regeneration tower (14) circularly flows between the tower bottom and the shell side or the tube side of the thermosiphon reboiler by utilizing the density difference, and the heat generated by the gas combustion of the heat conduction oil heating furnace a (18) is transferred to the tower bottom material of the regeneration tower through the thermosiphon reboiler.
3. An apparatus for producing a fine click as defined in claim 2, wherein: the static melting crystallizer (39) is mainly provided with a main device for static melting crystallization, wherein a finned tube structure is arranged inside a box body, a feed inlet and a discharge outlet are arranged at the bottom of the box body, the static melting crystallizer (39) is a static melting crystallizer (39) with a breathing tube orifice at the top, the box body is a cylinder or a tetragonal body, a jacket is arranged outside the box body, and three thermometers with different installation positions are arranged in the box body; the quality of the refined carbazole product can be effectively adjusted by adjusting the temperature at the end of crystallization cooling so as to meet different customer demands.
4. A process for producing high purity fine carbody by using the apparatus for producing fine carbody according to claim 1, comprising the steps of:
adding solvent oil into crude anthracene to melt in a crude anthracene melting tank (1), and sending the melted crude anthracene and solvent oil into a solvent crystallizer (5) after being cached in a crude anthracene caching tank (3), and cooling by using a primary cooler (9) and a deep cooler (10) for two steps of deep cooling until the temperature is reduced to 8 ℃; in the cooling process, the carboline and the anthracene are gradually crystallized and separated out, and phenanthrene and other impurities in the crude anthracene are discharged as mother liquor after crystallization together with solvent oil; mother liquor discharged from the solvent crystallizer (5) is sent to a solvent regeneration tower (14) after being buffered by a mother liquor buffer tank (12), solvent oil is recovered to a solvent oil storage tank (19) through distillation operation, and is sent to a melting tank (1) and a crude anthracene solvent proportioning tank (6) for recycling, and the regeneration tower residual liquor after solvent oil removal is used as a product to be sold to carbon black production or tar hydrogenation manufacturers; after the mother solution is discharged, fresh solvent oil is added into the solvent crystallizer (5) for a plurality of times, and the solvent oil is recrystallized for a plurality of times, and each recrystallization is subjected to the processes of adding the solvent oil, primary cooling, deep cooling and mother solution discharging; after the crystallization for many times is finished, filling solvent oil into a solvent crystallizer (5), heating to 120 ℃ by using a heater (11) to dissolve all crystals, conveying a mixture of carboline and the solvent oil after dissolving to a concentration tower (25) and an anthracene carboline distillation tower (31), distilling the solvent oil in the concentration tower (25) for recycling, conveying the anthracene carboline after concentration to the anthracene carboline distillation tower (31), and separating carboline from anthracene by reduced pressure distillation to obtain crude carbazole with 92% purity; finally, the crude carbazole is sent to a static melting crystallizer (39), and refined carboline with purity more than 98% is produced through static melting crystallization; the whole process except for transporting crude anthracene is automatically operated and completed in a DCS distributed control system.
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| CN201710068740.2A CN106995402B (en) | 2017-02-08 | 2017-02-08 | Equipment for producing fine-carbody and process for producing fine-carbody by utilizing static melting crystallization method |
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| CN201710068740.2A CN106995402B (en) | 2017-02-08 | 2017-02-08 | Equipment for producing fine-carbody and process for producing fine-carbody by utilizing static melting crystallization method |
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|---|---|---|---|---|
| CN108031141B (en) * | 2017-11-24 | 2020-09-25 | 孝感市易生新材料有限公司 | Process equipment and method for refining lactide |
| CN109535063B (en) * | 2019-01-15 | 2020-09-22 | 中钢集团鞍山热能研究院有限公司 | Process for extracting carbazole from anthracene oil by coupling separation method |
| KR20210151960A (en) * | 2019-04-15 | 2021-12-14 | 차이나 페트로리움 앤드 케미컬 코포레이션 | Method for separation of 2-alkylanthracene and use of 2-alkylanthracene for production of hydrogen peroxide |
| CN110272376B (en) * | 2019-07-19 | 2024-01-30 | 中冶焦耐(大连)工程技术有限公司 | Carbazole purification process, carbazole purification system and operation method of carbazole purification system |
| CN114522488A (en) * | 2021-12-25 | 2022-05-24 | 兖矿科蓝凯美特化工有限公司 | Workshop dust drainage washing processing system |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10103208A1 (en) * | 2001-01-24 | 2002-08-14 | Ruetgers Vft Ag | Obtaining anthracene and carbazole by melt crystallization |
| CN102516015A (en) * | 2011-12-12 | 2012-06-27 | 宝钢工程技术集团有限公司 | Production method and system for extracting refined anthracene and carbazole by using crystallization distillation method |
| CN103232318A (en) * | 2013-04-16 | 2013-08-07 | 中冶焦耐工程技术有限公司 | Method and device for producing refined anthracene, refined carbazole and phenanthrene product from raw material of monoanthracene oil |
| CN206751707U (en) * | 2017-02-08 | 2017-12-15 | 兖矿科蓝凯美特化工有限公司 | The equipment for producing smart click |
-
2017
- 2017-02-08 CN CN201710068740.2A patent/CN106995402B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10103208A1 (en) * | 2001-01-24 | 2002-08-14 | Ruetgers Vft Ag | Obtaining anthracene and carbazole by melt crystallization |
| CN102516015A (en) * | 2011-12-12 | 2012-06-27 | 宝钢工程技术集团有限公司 | Production method and system for extracting refined anthracene and carbazole by using crystallization distillation method |
| CN103232318A (en) * | 2013-04-16 | 2013-08-07 | 中冶焦耐工程技术有限公司 | Method and device for producing refined anthracene, refined carbazole and phenanthrene product from raw material of monoanthracene oil |
| CN206751707U (en) * | 2017-02-08 | 2017-12-15 | 兖矿科蓝凯美特化工有限公司 | The equipment for producing smart click |
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