CN115043697B - Industrial fluorene melting circulation drying method and drying system thereof - Google Patents
Industrial fluorene melting circulation drying method and drying system thereof Download PDFInfo
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- CN115043697B CN115043697B CN202210695718.1A CN202210695718A CN115043697B CN 115043697 B CN115043697 B CN 115043697B CN 202210695718 A CN202210695718 A CN 202210695718A CN 115043697 B CN115043697 B CN 115043697B
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- NIHNNTQXNPWCJQ-UHFFFAOYSA-N fluorene Chemical compound C1=CC=C2CC3=CC=CC=C3C2=C1 NIHNNTQXNPWCJQ-UHFFFAOYSA-N 0.000 title claims abstract description 148
- 238000002844 melting Methods 0.000 title claims abstract description 119
- 230000008018 melting Effects 0.000 title claims abstract description 117
- 238000001035 drying Methods 0.000 title claims abstract description 48
- 239000000463 material Substances 0.000 claims abstract description 64
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- 238000010438 heat treatment Methods 0.000 claims abstract description 47
- 238000009833 condensation Methods 0.000 claims abstract description 36
- 230000005494 condensation Effects 0.000 claims abstract description 36
- 239000007791 liquid phase Substances 0.000 claims abstract description 22
- 239000012071 phase Substances 0.000 claims abstract description 22
- 238000007599 discharging Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000013078 crystal Substances 0.000 claims abstract description 10
- 238000002425 crystallisation Methods 0.000 claims abstract description 5
- 230000008025 crystallization Effects 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 27
- 238000009434 installation Methods 0.000 claims description 15
- 239000000498 cooling water Substances 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- 239000010935 stainless steel Substances 0.000 claims description 8
- 238000003860 storage Methods 0.000 claims description 8
- 239000000155 melt Substances 0.000 claims description 6
- 238000004806 packaging method and process Methods 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000010865 sewage Substances 0.000 claims description 6
- 230000005484 gravity Effects 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 239000012808 vapor phase Substances 0.000 claims description 4
- 239000011229 interlayer Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000010309 melting process Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 20
- 239000011344 liquid material Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 210000001503 joint Anatomy 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000003983 fluorenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/09—Purification; Separation; Use of additives by fractional condensation
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B23/00—Heating arrangements
- F26B23/10—Heating arrangements using tubes or passages containing heated fluids, e.g. acting as radiative elements; Closed-loop systems
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
- F26B25/04—Agitating, stirring, or scraping devices
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2603/00—Systems containing at least three condensed rings
- C07C2603/02—Ortho- or ortho- and peri-condensed systems
- C07C2603/04—Ortho- or ortho- and peri-condensed systems containing three rings
- C07C2603/06—Ortho- or ortho- and peri-condensed systems containing three rings containing at least one ring with less than six ring members
- C07C2603/10—Ortho- or ortho- and peri-condensed systems containing three rings containing at least one ring with less than six ring members containing five-membered rings
- C07C2603/12—Ortho- or ortho- and peri-condensed systems containing three rings containing at least one ring with less than six ring members containing five-membered rings only one five-membered ring
- C07C2603/18—Fluorenes; Hydrogenated fluorenes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Water Supply & Treatment (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Analytical Chemistry (AREA)
- General Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Drying Of Solid Materials (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Abstract
The invention relates to the technical field of industrial fluorene processing, in particular to an industrial fluorene melting circulation drying method and a drying system thereof, wherein the industrial fluorene melting circulation drying method comprises a condensation cooler, an oil-water separator, a feeding device, a melting tank, a melting dryer, a slicing machine and a discharging device which are sequentially connected, a liquid-phase material outlet I of the melting tank is connected with a feeding port of the melting dryer, a liquid-phase material outlet II of the melting dryer is connected with a feeding pipeline of the slicing machine, a gas-phase material outlet I of the melting tank is connected with a gas-phase material inlet I of the condensation cooler, and a liquid-phase material outlet III of the condensation cooler is connected with a material inlet of an oil-water separator; the invention obtains the finished product industrial fluorene by melting, heating, desolventizing, dehydrating and slicing wet fluorene crystal particles produced in the industrial fluorene crystallization process under normal pressure or negative pressure. Compared with the prior art, the invention has the advantages of large treatment capacity, good drying effect and environmental protection.
Description
Technical Field
The invention relates to the technical field of industrial fluorene processing, in particular to an industrial fluorene melting and circulating drying method and a drying system thereof.
Background
The fluorene-rich fraction obtained by washing oil processing is crystallized and separated to obtain fluorene crystals, and the fluorene crystals contain certain moisture and solvent, which is called wet industrial fluorene; as a commodity, strict requirements are imposed on moisture and solvent content, and at present, a method for directly drying wet industrial fluorene crystal particles is widely adopted in industry to remove moisture and solvent. The prominent problems with this approach are: as the melting point of fluorene is 114.77 ℃, in order to prevent melting of fluorene in the drying process, drying can only be carried out at a lower temperature, hot water is used as a heating medium for drying, the drying temperature is generally controlled to be not more than 100 ℃, the boiling point of solvent in wet industrial fluorene is 135-145 ℃, the stripping effect of water and solvent is poor due to the fact that the temperature control is low, the market requirement is not met, the condition that fluorene crystal particles cannot be normally produced due to melting of the temperature control is high, and the production is seriously influenced. In order to improve the drying effect and meet the market demand, many enterprises take the following measures in the industrial fluorene drying process: reducing the treatment capacity; introducing inert gas into the dryer; and (5) performing secondary drying. The following problems exist in the above measures: introducing inert gas into the dryer, and discharging tail gas to pollute the environment; reducing throughput and performing secondary drying can affect yield; when industrial fluorene with lower moisture content is required in the market, the above measures still cannot meet the requirements, and the drying of the industrial fluorene becomes a bottleneck in the industrial fluorene production process.
Therefore, there is a need to develop a novel wet industrial fluorene drying process to solve the problem of poor solvent removal and dehydration effects of wet industrial fluorene and the influence on the environment.
Disclosure of Invention
In order to overcome the defects existing in the prior art, the industrial fluorene melting circulation drying method and the drying system thereof with good drying effect, large processing capacity and environmental protection are provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
an industrial fluorene melt cycle drying method comprising:
s1, conveying wet industrial fluorene crystals generated in an industrial fluorene crystallization process to a melting tank for heating and melting;
s2, the melted wet industrial fluorene flows to a melting dryer by means of potential difference, a stirrer, a heating tube bundle and a central tube are sequentially arranged in the melting dryer from top to bottom, the liquid industrial fluorene forcedly flows under the action of the stirrer and flows into the heating tube bundle and the central tube, and natural flow is formed due to different heating degrees, so that solvents and moisture are removed;
s3, enabling vapor phase materials at the tops of the melting tank and the melting dryer to enter a condensation cooler through a pipeline to be condensed and cooled into a mixed solution of water and solvent; the mixed liquid automatically flows into an oil-water separator by the potential difference; standing and separating by specific gravity difference, and enabling the separated solvent to automatically flow to a solvent storage tank by the specific gravity difference for recycling; the separated water enters a sewage treatment device;
s4, enabling partial droplets of uncondensed gas materials in the condensation cooler to enter a vacuum tank and be captured, and then sending the droplets into an oil-water separator to perform oil-water separation together with mixed liquid condensed and cooled by the condensation cooler; the noncondensable gas in the vacuum tank is conveyed to a tail gas treatment system for treatment through a vacuum pump;
s5, the industrial fluorene with the solvent and the moisture removed automatically flows to the bottom of the slicer by means of the level difference, is solidified and cut into slices, and is packaged and put in storage.
Preferably, the melting temperature of the melting tank is 120-140 ℃, and the pressure of the melting tank is 0KPa to minus 60KPa.
Preferably, the melt dryer has a drying temperature of 130-180deg.C and a drying pressure of 0KPa to minus 60KPa.
Preferably, the commercial fluorene is left in the melt dryer for a residence time of 2-6 hours.
An industrial fluorene melting circulation drying system comprises a condensation cooler, an oil-water separator, a feeding device, a melting tank, a melting dryer, a slicing machine and a discharging device which are connected in sequence; the liquid phase material outlet I of the melting tank is connected with the feeding port of the melting dryer, and the liquid phase material outlet II of the melting dryer is connected with the feeding pipeline of the slicer; the gas-phase material outlet I of the melting tank is connected with the gas-phase material inlet I of the condensation cooler, the liquid-phase material outlet III of the condensation cooler is connected with the material inlet of the oil-water separator, and a cooling water pipeline I is arranged in the condensation cooler.
For further optimization, the oil-water separator further comprises a vacuum tank, wherein a gas-phase material inlet II of the vacuum tank is communicated with a gas-phase material outlet II of the condensation cooler, and a liquid-phase material outlet IV of the vacuum tank is connected with a material inlet of the oil-water separator.
In order to realize melting and drying, a heating coil I is arranged in the melting tank, heating medium of the heating coil I is steam or heat conducting oil, a heating coil II and a stirrer are arranged in the melting dryer, and heating medium of the heating coil II is steam or heat conducting oil;
the feeding device and the discharging device are both pipe chain type conveyors, the feeding end of the feeding device is arranged on the ground, and the discharging end of the discharging device is connected with a packaging unit; the melting dryer is internally provided with a stirrer, a heating tube bundle and a central tube, and the sectional area of the central tube is 40% -60% of that of the melting dryer.
In order to recycle the separated solvent, a solvent oil outlet pipeline of the oil-water separator is connected with a solvent oil storage tank, and a separation water outlet pipeline of the oil-water separator is connected with a sewage treatment system.
Further, the installation height of the melting tank is 10-12 m, the installation height of the melting dryer is 6.5-8.5 m, and the slicer is installed on the ground;
the installation height of the condensation cooler is 9-11 m, the installation height of the oil-water separator is 4-6 m, and the installation height of the vacuum tank is 9-11 m.
Further, the slicing machine is made of stainless steel, a cooling water pipeline is arranged in the slicing machine, a liquid sealing device is arranged at the inlet of a receiving disc of the slicing machine, and a heating interlayer is arranged at the bottom of the receiving disc;
the vacuum tank is connected with a vacuum pump, the vacuum pump is installed on the ground, and an outlet pipeline of the vacuum pump is connected with the tail gas treatment system.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts the melting dryer to carry out dehydration and desolventizing under negative pressure and higher temperature, has flexible operation, good drying effect, improves the processing capacity, improves the quality of finished industrial fluorene, has no nitrogen entering into the system in the drying process and has little environmental pollution. And crystallizing fluorene-rich components obtained in the distillation process of the distillate oil of the high-temperature coal tar at 230-300 ℃ to obtain wet industrial fluorene, dehydrating residual solvent and moisture in the wet industrial fluorene by using a melting heating method, and slicing and packaging the liquid industrial fluorene from which the solvent and the moisture are removed.
2. Compared with the prior art, the industrial fluorene melting and drying production process has the advantages of high automation level, simplicity in operation, high yield, environmental protection and the like; the industrial fluorene moisture content is reduced from 1.0% to 0.3%, and the effect is very obvious.
Drawings
The following detailed description of the invention will be given with reference to the accompanying drawings.
FIG. 1 is a schematic diagram of the structure of the present invention;
fig. 2 is a partial enlarged view of a in fig. 1.
In the figure: 1-feeding device, 2-melting tank, 21-gas phase material outlet I, 22-heating coil I, 23-liquid phase material outlet I, 3-melting dryer, 31-liquid phase material outlet II, 4-slicer, 5-discharging device, 6-condensing cooler, 61-gas phase material inlet I, 62-liquid phase material outlet III, 63-cooling water pipeline I, 64-gas phase material outlet II, 7-oil-water separator, 71-material inlet, 72-solvent oil outlet pipeline, 73-separating water outlet pipeline, 8-vacuum tank, 81-gas phase material inlet II, 82-liquid phase material outlet IV, 9-vacuum pump, 91-outlet pipeline.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
as shown in fig. 1 to 2, an industrial fluorene melt cycle drying method includes:
s1, conveying wet industrial fluorene obtained after a fluorene crystallization process to a melting tank 2 by a pipe chain conveyor, wherein a heating coil is arranged in the melting tank 2, steam or heat conducting oil is introduced into the heating coil, and the wet industrial fluorene in the melting tank 2 is indirectly heated and melted;
s2, automatically flowing molten wet industrial fluorene leaning head from a melting tank 2 to a melting dryer 3, wherein a stirrer, a heating tube bundle and a central tube are arranged in the melting dryer 3; the liquid industrial fluorene is forced to flow under the action of a stirrer at the upper part of the melting dryer 3, and the liquid industrial fluorene forms natural flow under different heating degrees in the heating tube bundle and the central tube at the lower part of the melting dryer 3, so that the solvent and the moisture in the wet industrial fluorene are heated and vaporized under the stirring state;
s3, the vapor phase materials at the tops of the melting tank 2 and the melting dryer 3 are mixed vapor of solvent and water, the mixed vapor enters a condensation cooler 6 and is condensed and cooled, the condensed and cooled water and solvent mixed liquid automatically flows to an oil-water separator 7 through the bottom of the condensation cooler 6 by potential difference, the mixed liquid is subjected to standing separation in the oil-water separator 7 by the potential difference, and the separated solvent automatically flows to a solvent storage tank by the potential difference for recycling; the separated water enters a sewage treatment device;
s4, enabling partial liquid drops carried by the gas materials which are not condensed in the condensation cooler 6 to enter the vacuum tank 8, capturing the carried liquid drops in the vacuum tank 8, entering the oil-water separator 7 through the bottom liquid material outlet, and carrying out oil-water separation together with the mixed liquid at the bottom of the condensation cooler 6; the noncondensable gas of the vacuum tank 8 is conveyed to a tail gas treatment system for treatment through a vacuum pump 9.
S5, the industrial fluorene with solvent and moisture removed automatically flows to the bottom of the slicer 4 by the position difference from the melting dryer 3, the liquid industrial fluorene is cooled and solidified by the slicer 4 and cut into slices, and the slices are conveyed to a packaging unit by a finished product industrial fluorene pipe chain conveyor, and packaged, transported for warehouse entry or delivered from a factory.
The melting tank 2 is made of stainless steel, and the heating medium is steam or heat conducting oil; the melting industrial fluorene pipe from the melting tank to the melting dryer 3 is made of stainless steel. The melting dryer 3 is made of stainless steel, and the heating medium is steam or heat conducting oil; the industrial fluorene pipeline from the melting dryer 3 to the slicing machine 4 after drying is made of stainless steel. The slicer 4 is made of stainless steel, a heating interlayer is arranged at the bottom of the receiving tray, heating medium is steam or heat conducting oil, and cooling medium is circulating water.
The melting temperature of the melting tank is 120-140 ℃, the pressure of the melting tank is 0KPa to minus 60KPa, the drying temperature of the melting dryer is 130-180 ℃, the drying pressure is 0KPa to minus 60KPa, the rotating speed of the stirrer in the melting dryer 3 is 20-60r/min, and the cross section area of the central tube of the melting dryer is 40-60 percent, preferably 50 percent of the cross section area of the melting dryer 3; the residence time of the material in the melt dryer 3 is 2 to 6 hours, preferably 4 hours; the temperature of the mixed solution cooled by the condensation cooler 6 is less than 40 ℃.
Example 2:
as shown in fig. 1 and fig. 2, a melting method industrial fluorene drying system can be applied to an industrial fluorene melting circulation drying method in embodiment 1, and the melting method comprises a feeding device 1, a melting tank 2, a melting dryer 3, a slicer 4, a discharging device 5, a condensation cooler 6, an oil-water separator 7 and a vacuum tank 8 which are sequentially connected, wherein the feeding device 1 and the discharging device 5 are all of a tube chain type conveyor, the feeding end of the feeding device 1 is arranged on the ground, the discharging end is in butt joint with the melting tank, the feeding end of the discharging device 5 is in butt joint with the slicer 4, and the discharging end of the discharging device 5 can be connected with a packaging unit to realize automatic packaging.
The melting tank 2 is used for melting wet industrial fluorene crystals with the moisture content of about 2% from a fluorene crystallization process, the upper end of the melting tank 2 is provided with a material inlet and a gas-phase material outlet I21, the wet industrial fluorene crystals enter the material inlet of the melting tank 2 through the feeding device 1, a heating coil I22 is arranged in the melting tank 2, inlet and outlet connecting pipes of the heating coil I22 are respectively connected with a heating medium inlet and outlet pipeline, heating medium of the heating coil I22 can adopt steam or heat conducting oil and the like, the wet industrial fluorene crystals are melted through the heating coil I22, the temperature is 130 ℃, the pressure is 30KPa, and the lower end of the melting tank 2 is provided with a liquid-phase material outlet I23.
The upper end of the melting dryer 3 is provided with a feed inlet and a gas-phase material outlet, the feed inlet is communicated with the liquid-phase material outlet I of the melting tank 2, a heating coil II 32 and a stirrer 33 are arranged in the melting dryer 3, a heating medium of the heating coil II 32 is steam or heat conduction oil, the melting dryer 3 is dried under the conditions of 150 ℃ and 30KPa and stirring, the moisture content is reduced to below 0.5%, and the lower end of the melting dryer 3 is provided with the liquid-phase material outlet II 31.
The slicer 4 is stainless steel, is provided with the cooling water pipeline in the slicer 4, and the receiving plate entrance of slicer 4 is provided with the liquid seal device, and receiving plate bottom is provided with the heating intermediate layer. The liquid phase material outlet II 31 of the melting dryer is connected with the liquid sealing device, and the material enters the receiving tray through the liquid sealing device, and enters the discharging device 5 after being solidified and sliced.
The installation height of the melting tank 2 is 10-12 m, the installation height of the melting dryer 3 is 6.5-8.5 m, the slicer 4 is installed on the ground, and the liquid materials among the melting tank 2, the melting dryer 3 and the slicer 4 are automatically flowed by means of level difference.
In the figure, a is a heat medium inlet, and b is a heat medium outlet; c is a cooling water inlet, and d is a cooling water outlet.
The gas phase material outlet I21 of the melting tank 2 and the gas phase material outlet of the melting dryer are connected with the gas phase material inlet I61 of the condensation cooler 6, a cooling water pipeline I63 is arranged in the condensation cooler 6, the gas phase materials at the tops of the melting tank 2 and the melting dryer 3 enter the condensation cooler 6 to be condensed and cooled, and the condensed and cooled liquid materials are mixed liquid of water and solvent.
The liquid phase material outlet III 62 of the condensation cooler 6 is connected with the material inlet 71 of the oil-water separator 7, the mixed liquid flows into the oil-water separator 7 by the potential difference from the bottom of the condensation cooler 6, the mixed liquid is subjected to standing separation by the potential difference, the separated solvent flows into the solvent storage tank by the potential difference for recycling, and the separated water enters the sewage treatment device.
The gas-phase material inlet II 81 of the vacuum tank 8 is communicated with the gas-phase material outlet II 64 of the condensation cooler 6, and the liquid-phase material outlet IV 82 of the vacuum tank 8 is connected with the material inlet 71 of the oil-water separator 7. The uncondensed gas material of the condensation cooler 6 carries part of liquid drops into the vacuum tank 8, the carried liquid drops are captured in the vacuum tank 8, enter the oil-water separator from the bottom liquid material outlet, and are separated with the mixed liquid at the bottom of the condensation cooler 6; the vacuum tank 8 is connected with a vacuum pump 9, the vacuum pump 9 is installed on the ground, an outlet pipeline 91 of the vacuum pump 9 is connected with the tail gas treatment system, and noncondensable gas of the vacuum tank 8 is conveyed to the tail gas treatment system for treatment through the vacuum pump.
The installation height of the condensation cooler 6 is 9-11 m, the installation height of the oil-water separator 7 is 4-6 m, the installation height of the vacuum tank 8 is 9-11 m, and liquid phase materials for cooling the condenser 6 and the oil-water separator 7 automatically flow into the oil-water separator through level difference.
The preferred embodiments of the present invention have been described in detail, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention, and the various changes are included in the scope of the present invention.
Claims (8)
1. An industrial fluorene melting and circulating drying method is characterized by comprising the following steps:
s1, conveying wet industrial fluorene crystals generated in an industrial fluorene crystallization process to a melting tank (2) for heating and melting;
s2, enabling the melted wet industrial fluorene to flow to a melting dryer (3) by means of a potential difference, sequentially installing a stirrer, a heating tube bundle and a central tube in the melting dryer (3) from top to bottom, forcibly flowing liquid industrial fluorene under the action of the stirrer, flowing the liquid industrial fluorene into the heating tube bundle and the central tube, forming natural flow due to different heating degrees, and removing solvent and moisture;
s3, enabling vapor phase materials at the tops of the melting tank (2) and the melting dryer (3) to enter a condensation cooler (6) through a pipeline, and condensing and cooling the vapor phase materials into a mixed solution of water and solvent; the mixed liquid automatically flows into an oil-water separator (7) by the potential difference; standing and separating by specific gravity difference, and enabling the separated solvent to automatically flow to a solvent storage tank by the specific gravity difference for recycling; the separated water enters a sewage treatment device;
s4, enabling partial droplets carried by uncondensed gas materials in the condensation cooler (6) to enter a vacuum tank (8) and be captured, and then sending the droplets into an oil-water separator (7) to carry out oil-water separation together with mixed liquid condensed and cooled by the condensation cooler (6); the noncondensable gas in the vacuum tank (8) is conveyed to a tail gas treatment system for treatment through a vacuum pump;
s5, the industrial fluorene with the solvent and the moisture removed automatically flows to the bottom of the slicer (4) by means of the level difference, is cooled, solidified and cut into slices, and is packaged and put in storage.
2. An industrial fluorene melt circulation drying method as claimed in claim 1, characterized in that the melting temperature of the melting tank (2) is 120-140 ℃, and the pressure of the melting tank (2) is 0KPa to minus 60KPa.
3. An industrial fluorene melt circulation drying method as claimed in claim 1 or 2, characterized in that the melt dryer (3) has a drying temperature of 130-180 ℃ and a drying pressure of 0KPa to minus 60KPa.
4. Process for the melt cycle drying of industrial fluorene according to claim 1 or 2, characterized in that the residence time of said industrial fluorene in the melt dryer (3) is 2-6 hours.
5. The industrial fluorene melting circulation drying system is characterized by comprising a condensation cooler (6), an oil-water separator (7), a feeding device (1), a melting tank (2), a melting dryer (3), a slicing machine (4) and a discharging device (5) which are sequentially connected, wherein a liquid-phase material outlet I (23) of the melting tank (2) is connected with a feeding hole of the melting dryer (3), and a liquid-phase material outlet II (31) of the melting dryer (3) is connected with a feeding pipeline of the slicing machine (4); the gas-phase material outlet I (21) of the melting tank (2) is connected with the gas-phase material inlet I (61) of the condensation cooler (6), the liquid-phase material outlet III (62) of the condensation cooler (6) is connected with the material inlet (71) of the oil-water separator (7), and a cooling water pipeline I (63) is arranged in the condensation cooler (6);
the device also comprises a vacuum tank (8), wherein a gas-phase material inlet II (81) of the vacuum tank (8) is communicated with a gas-phase material outlet II (64) of the condensation cooler (6), and a liquid-phase material outlet IV (82) of the vacuum tank (8) is connected with a material inlet (71) of the oil-water separator (7);
a heating coil I (22) is arranged in the melting tank (2), a heating medium of the heating coil I (22) is steam or heat conduction oil, a heating coil II (32) and a stirrer (33) are arranged in the melting dryer (3), and the heating medium of the heating coil II (32) is steam or heat conduction oil;
the feeding device (1) and the discharging device (5) are both pipe chain type conveyors, the feeding end of the feeding device (1) is arranged on the ground, and the discharging end of the discharging device (5) is connected with a packaging unit; the melting dryer (3) is internally provided with a stirrer, a heating tube bundle and a central tube, and the sectional area of the central tube is 40% -60% of that of the melting dryer.
6. The melting industrial fluorene drying system as claimed in claim 5, wherein the solvent oil outlet pipe (72) of the oil-water separator (7) is connected with a solvent oil storage tank, and the separated water outlet pipe (73) of the oil-water separator (7) is connected with a sewage treatment system.
7. A melting process industrial fluorene drying system as claimed in claim 5, characterized in that the installation height of the melting tank (2) is 10-12 m, the installation height of the melting dryer (3) is 6.5-8.5 m, and the slicer (4) is installed on the ground;
the installation height of the condensation cooler (6) is 9-11 m, the installation height of the oil-water separator (7) is 4-6 m, and the installation height of the vacuum tank (8) is 9-11 m.
8. The melting method industrial fluorene drying system according to claim 5, wherein the slicing machine (4) is made of stainless steel, a cooling water pipeline is arranged in the slicing machine (4), a liquid sealing device is arranged at the inlet of a receiving tray of the slicing machine (4), and a heating interlayer is arranged at the bottom of the receiving tray;
the vacuum tank (8) is connected with a vacuum pump (9), the vacuum pump (9) is installed on the ground, and an outlet pipeline (91) of the vacuum pump (9) is connected with the tail gas treatment system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210695718.1A CN115043697B (en) | 2022-06-20 | 2022-06-20 | Industrial fluorene melting circulation drying method and drying system thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09157188A (en) * | 1995-12-11 | 1997-06-17 | Nippon Shokubai Co Ltd | Production of fluorene |
| CN1884234A (en) * | 2005-06-22 | 2006-12-27 | 上海宝钢化工有限公司 | Method for purifying fluorene crystals |
| CN101182278A (en) * | 2007-12-12 | 2008-05-21 | 卫宏远 | Method for purifying refined fluorene by crystallizing process |
| CN103304365A (en) * | 2013-06-28 | 2013-09-18 | 江西理工大学 | New process for purifying and refining coarse fluorene |
| CN103936544A (en) * | 2014-01-07 | 2014-07-23 | 成都科特瑞兴科技有限公司 | Novel apparatus for purifying crude fluorene fraction |
-
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- 2022-06-20 CN CN202210695718.1A patent/CN115043697B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09157188A (en) * | 1995-12-11 | 1997-06-17 | Nippon Shokubai Co Ltd | Production of fluorene |
| CN1884234A (en) * | 2005-06-22 | 2006-12-27 | 上海宝钢化工有限公司 | Method for purifying fluorene crystals |
| CN101182278A (en) * | 2007-12-12 | 2008-05-21 | 卫宏远 | Method for purifying refined fluorene by crystallizing process |
| CN103304365A (en) * | 2013-06-28 | 2013-09-18 | 江西理工大学 | New process for purifying and refining coarse fluorene |
| CN103936544A (en) * | 2014-01-07 | 2014-07-23 | 成都科特瑞兴科技有限公司 | Novel apparatus for purifying crude fluorene fraction |
Non-Patent Citations (3)
| Title |
|---|
| 利用熔融结晶法进行芴的提纯;贾春燕 等;化工学报;第58卷(第09期);第2266-2269页 * |
| 熔融结晶技术研究及应用进展;钟伟 等;中外能源;第15卷(第06期);第95-99页 * |
| 芴的提取精制研究进展;李素梅 等;河北化工(第06期);第14-15、64页 * |
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