CN115245789A - Phenol extraction device capable of operating for long time - Google Patents
Phenol extraction device capable of operating for long time Download PDFInfo
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- CN115245789A CN115245789A CN202111562021.9A CN202111562021A CN115245789A CN 115245789 A CN115245789 A CN 115245789A CN 202111562021 A CN202111562021 A CN 202111562021A CN 115245789 A CN115245789 A CN 115245789A
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- phenol
- cold trap
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- trap device
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 title claims abstract description 190
- 238000000605 extraction Methods 0.000 title claims abstract description 23
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims abstract description 128
- 238000010438 heat treatment Methods 0.000 claims abstract description 128
- 238000005507 spraying Methods 0.000 claims abstract description 48
- 238000004140 cleaning Methods 0.000 claims abstract description 47
- 239000011229 interlayer Substances 0.000 claims abstract description 39
- 238000009833 condensation Methods 0.000 claims abstract description 33
- 230000005494 condensation Effects 0.000 claims abstract description 33
- 238000003860 storage Methods 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 230000007774 longterm Effects 0.000 claims abstract description 8
- 239000011261 inert gas Substances 0.000 claims description 24
- 239000007787 solid Substances 0.000 claims description 21
- 238000009835 boiling Methods 0.000 claims description 3
- 230000008014 freezing Effects 0.000 claims description 3
- 238000007710 freezing Methods 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims 3
- 239000004417 polycarbonate Substances 0.000 abstract description 9
- 229920000515 polycarbonate Polymers 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 229920000642 polymer Polymers 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 150000003384 small molecules Chemical class 0.000 description 12
- 238000000034 method Methods 0.000 description 11
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 238000013461 design Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000004888 barrier function Effects 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- -1 phenol in the tank Chemical class 0.000 description 3
- 238000006068 polycondensation reaction Methods 0.000 description 3
- 241000521257 Hydrops Species 0.000 description 2
- 206010030113 Oedema Diseases 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000005809 transesterification reaction Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 208000035475 disorder Diseases 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D8/00—Cold traps; Cold baffles
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G64/00—Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
- C08G64/04—Aromatic polycarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G64/00—Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
- C08G64/20—General preparatory processes
- C08G64/30—General preparatory processes using carbonates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0869—Feeding or evacuating the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0871—Heating or cooling of the reactor
Abstract
The invention discloses a phenol extraction device capable of operating for a long time. The device comprises a cleaning solution storage tank, a first cold hydrazine device, a phenol collecting tank and a second cold hydrazine device, wherein the cleaning solution storage tank is positioned above the first cold hydrazine device, and the second cold hydrazine device is arranged on the side of the phenol collecting tank; the bottom of the cleaning solution storage tank is communicated with a first cold hydrazine device, the bottom of the first cold hydrazine device is respectively communicated with a phenol collecting tank, and the phenol collecting tank is communicated with a second cold hydrazine device; the two cold hydrazine devices are the same in layout, a condensation jacket is arranged on the outer wall, a heating bottom shell is arranged on the lower side, and an interlayer and a spraying device connected with a cleaning liquid storage tank are arranged inside the cold hydrazine devices. The invention can avoid the pipeline blockage while ensuring the phenol is completely extracted, protect the pump body from being damaged by the phenol, reduce the vacuum fluctuation, maintain the long-term operation of the device, and is suitable for the devolatilization acquisition of the phenol and other micromolecules in the production process of polymers such as polycarbonate and the like.
Description
Technical Field
The invention relates to a poisonous and corrosive liquid extraction device, in particular to a phenol extraction device capable of operating for a long time.
Background
In recent years, aromatic polycarbonates have been widely used in various fields as engineering plastics having excellent properties in heat resistance, impact resistance, transparency, and the like. The industrial production methods of polycarbonates are largely classified into two methods, phosgene method and melt polycondensation method. Among them, the melt polycondensation method is widely carried out due to the characteristics of no solvent, greenness, energy saving and less impurities.
The melt polycondensation process for producing aromatic polycarbonates is a reversible reaction, and transesterification reactions produce large amounts of phenol. The normal synthesis of polycarbonate can be promoted only by continuously extracting the generated phenol while maintaining a vacuum system in the reaction. The melting point of the phenol is 43 ℃, the phenol is a crystalline solid at normal temperature, and if the process is improperly controlled in the extraction process, the phenol is easy to solidify and block a pipeline to cause system vacuum disorder; phenol is also corrosive and if collected incompletely into the oil pump cavity, the pump body will be damaged after a long time. The clogging of the piping and the damage to the pump body by phenol lead to the abnormality in the production of polycarbonate.
Therefore, a reliable phenol extraction device is needed, so that the complete extraction of phenol is ensured while the pipeline is prevented from being blocked, and the long-term operation of production equipment is ensured.
Disclosure of Invention
In order to overcome the problems in the background art, the invention aims to provide a phenol extraction device capable of operating for a long time.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problem is as follows:
the cleaning solution storage tank is positioned above the side of the first cold hydrazine device, and the second cold hydrazine device is arranged on the side of the phenol collection tank; the bottom of the cleaning solution storage tank is communicated with a first cold hydrazine device, the bottom of the first cold hydrazine device is respectively communicated with a phenol collecting tank, and the phenol collecting tank is communicated with a second cold hydrazine device.
In the first cold trap apparatus: the outer wall of the upper middle part of the first cold trap device is provided with a first condensation jacket, and the first condensation jacket is used for condensing the gaseous phenol falling to the upper middle part of the first cold trap device to form a liquid state or a solid state; the lower part of the first cold trap device is provided with a first heating bottom shell, and the first heating bottom shell is used for heating liquid phenol or solid phenol falling to the lower part of the first cold trap device to obtain liquid phenol; a vertically arranged first interlayer is fixedly arranged in the middle of the inner top surface between the two sides of the first cold hydrazine device, the upper end of the first interlayer is fixedly and hermetically connected with the inner top surface of the first cold hydrazine device, and the lower end of the first interlayer extends downwards to the outlet at the bottom end of the first cold hydrazine device, so that the inner cavity of the first cold hydrazine device is divided into two local inner cavities at the two sides;
in the second cold trap device: the outer wall of the upper middle part of the second cold trap device is provided with a second condensation jacket, and the second condensation jacket is used for condensing the gaseous phenol falling to the upper middle part of the second cold trap device to form a liquid state or a solid state; the lower part of the second cold hydrazine device is provided with a second heating bottom shell, and the second heating bottom shell is used for heating liquid phenol or solid phenol falling to the lower part of the second cold hydrazine device to form liquid phenol; and a vertically arranged second interlayer is fixedly arranged in the middle of the inner top surface between the two sides of the second cold hydrazine device, the upper end of the second interlayer is fixedly and hermetically connected with the inner top surface of the second cold hydrazine device, and the lower end of the second interlayer extends downwards to the outlet at the bottom end of the second cold hydrazine device, so that the inner cavity of the second cold hydrazine device is divided into two local inner cavities at the two sides.
In the first cold trap apparatus: an airflow inlet channel and an airflow outlet channel extend upwards from two sides of the first cold trap device divided by the first interlayer, the airflow inlet channel is communicated with a first inlet heating pipeline which is continuously input and mainly takes gaseous phenol, and the airflow outlet channel is communicated with a first outlet heating pipeline; the first outlet heating pipeline is communicated with an inlet of a first vacuum pump; an outlet at the bottom of the cleaning solution storage tank is respectively communicated with an airflow inlet channel and an airflow outlet channel of the first cold trap device through a first valve and a second valve; and the top surfaces in two sides of the first cold trap device after the first interlayer is divided are respectively provided with a first spraying device and a second spraying device, and inlets of the first spraying device and the second spraying device are respectively communicated with an outlet at the bottom of the cleaning solution storage tank.
In the second cold trap device: an airflow inlet channel and an airflow outlet channel extend outwards from two sides of the second cold trap device divided by the second interlayer, the airflow inlet channel is communicated with a second inlet heating pipeline which mainly inputs inert gas, and the airflow outlet channel is communicated with a second outlet heating pipeline; the second outlet heating pipeline is communicated with an inlet of a second vacuum pump through a seventh valve; and the inner top surfaces of two sides of the second cold trap device after the second interlayer division are respectively provided with a third spraying device and a fourth spraying device, and inlets of the third spraying device and the fourth spraying device are respectively communicated with an outlet at the bottom of the cleaning liquid storage tank.
The outlet at the bottom end of the first cold trap device is respectively communicated with an inert gas supply port, a phenol collecting tank and a second inlet heating pipeline through a four-way joint; and a port for phenol circulation is arranged in the middle of the phenol collecting tank, is obliquely and upwards arranged and is communicated with an outlet at the bottom end of the second cold trap device after passing through the eighth valve.
The first cold hydrazine device and the phenol collecting tank are respectively connected to the upper end and the lower end of the cross joint, and the inert gas supply port and the second inlet heating pipeline are respectively connected to ports on two horizontal sides of the cross joint.
The outlet at the bottom end of the first cold hydrazine device is connected with the four-way valve through a third valve, the inert gas supply port is connected with the four-way valve through a fourth valve, the second inlet heating pipeline is connected with the four-way valve through a fifth valve, and the phenol collecting tank is directly connected with the four-way valve.
And an outlet at the bottom of the phenol collecting tank is communicated with a phenol discharge port through a sixth valve.
The first inlet heating pipeline, the first outlet heating pipeline, the first heating bottom shell, the second inlet heating pipeline, the second outlet heating pipeline, the second heating bottom shell, the phenol collecting tank and the outer wall of the phenol direct contact fitting are all provided with heating fitting jackets.
In the cleaning solution storage tank, the boiling point of the cleaning solution is higher than the temperatures of a first inlet heating pipeline, a first outlet heating pipeline, a first heating bottom shell, a second inlet heating pipeline, a second outlet heating pipeline, a second heating bottom shell and heating accessories in the phenol collecting tank, and the freezing point is lower than the temperatures of the first condensation jacket and the second condensation jacket.
The invention has the following beneficial effects:
according to the invention, by effectively heating the extraction pipeline and effectively condensing small molecules such as phenol and the like and matching with the use of the cleaning solution, vacuum instability caused by pipeline blockage due to solidification of the small molecules such as phenol and the like can be avoided, phenol can be efficiently extracted, and the vacuum pump is prevented from being damaged by phenol.
The invention can avoid the pipeline blockage while ensuring the phenol is completely extracted, protect the pump body from being damaged by the phenol, reduce the vacuum fluctuation, maintain the long-term operation of the device, and is suitable for the devolatilization acquisition of the phenol and other micromolecules in the production process of polymers such as polycarbonate and the like.
The device has reasonable structure, can be used singly or in series, and can effectively maintain the long-term production of the aromatic polycarbonate production device.
Drawings
The invention is further illustrated with reference to the following figures and examples.
Fig. 1 is a schematic view of an assembly structure according to an embodiment of the present invention.
The numbers in the figure represent: 1. the cleaning solution storage tank comprises a cleaning solution storage tank, 2, a first valve, 3, a first inlet heating pipeline, 4, a first spraying device, 5, a first cold trap device, 6, a first condensation jacket, 7, a first interlayer, 8, a first heating bottom shell, 9, a fourth valve, 10, an inert gas supply port, 11, a phenol collection tank, 12, a phenol discharge port, 13, a sixth valve, 14, a second inlet heating pipeline, 15, a fifth valve, 16, a third valve, 17, a second spraying device, 18, a first outlet heating pipeline, 19, a second valve, 20, a first vacuum pump, 21, a second vacuum pump, 22, a third spraying device, 23, a fourth spraying device, 24, a second outlet heating pipeline, 25, a seventh valve, 26, a second condensation jacket, 27, a second cold trap device, 28, a second interlayer, 29, a second heating bottom shell and 30, and an eighth valve.
Detailed Description
The invention is further described with reference to the accompanying drawings and the detailed description.
In this example, a phenol extraction apparatus capable of operating for a long time shown in FIG. 1 was used to continuously extract small molecules such as phenol generated in the production of polycarbonate by the melt transesterification method.
The phenol extraction device capable of operating for a long time provided by the embodiment comprises a cleaning solution storage tank 1, a first cold trap device 5, a phenol collection tank 11 and a second cold trap device 27, wherein the cleaning solution storage tank 1 is positioned above the side of the first cold trap device 5, and the second cold trap device 27 is arranged on the side of the phenol collection tank 11; the bottom of the cleaning solution storage tank 1 is communicated with the first cold hydrazine device 5, the bottom of the first cold hydrazine device 5 is respectively communicated with the phenol collecting tank 11, and the phenol collecting tank 11 is communicated with the second cold hydrazine device 27.
The cleaning solution storage tank 1 is filled with a cleaning solution which is used for dissolving phenol and is in a liquid state and has a lower melting point.
Gaseous phenol enters the first cold trap device 5, is condensed and heated to become liquid phenol, then flows into the phenol collecting tank 11, is isolated from the first cold trap device 5 when the liquid in the phenol collecting tank 11 is filled to exceed the limit, and is discharged out under the normal pressure condition from the phenol collecting tank 11. After the discharge, the phenol collection tank 11 is connected to a second vacuum system manufactured by a second vacuum pump 21 by a second cold trap device 27 so that the pressure in the phenol collection tank 11 is changed from the normal pressure to the same pressure as the first cold trap device 5, and further phenol is output from the first cold trap device 5 to the phenol collection tank 11 and collected, and the discharged phenol is recovered to the phenol collection tank 11 by the second cold trap device 27 as necessary.
The outer wall of the upper middle part of the first cold trap device 5 is provided with a first condensation jacket 6, and the first condensation jacket 6 is used for condensing the gaseous phenol falling to the upper middle part of the first cold trap device 5 to form a liquid state or a solid state;
the lower part of the first cold trap device 5 is provided with a first heating bottom shell 8, and the first heating bottom shell 8 is used for heating the liquid phenol or the solid phenol falling to the lower part of the first cold trap device 5 to obtain the liquid phenol;
a vertically arranged first interlayer 7 is fixedly arranged in the middle of the inner top surface between the two sides of the first cold hydrazine device 5, the upper end of the first interlayer 7 is fixedly and hermetically connected with the inner top surface of the first cold hydrazine device 5, and the lower end of the first interlayer 7 extends downwards to an outlet at the bottom end of the first cold hydrazine device 5 and is lower than the first condensation jacket 6, so that the inner cavity of the first cold hydrazine device 5 is divided into two local inner cavities at the two sides;
the two sides of the first cold trap device 5 divided by the first interlayer 7 extend upwards to form an airflow inlet channel and an airflow outlet channel, the airflow inlet channel and the airflow outlet channel are positioned at the two sides of the first interlayer 7, the airflow inlet channel is used for introducing mixed gas of gaseous phenol and a very small amount of oligomer, the airflow outlet channel is used for allowing inert gas such as nitrogen filled in a reaction system before flowing out, the airflow inlet channel is communicated with a first inlet heating pipeline 3 which is mainly continuously input gaseous phenol, and the airflow outlet channel is communicated with a first outlet heating pipeline 18; the first outlet heated conduit 18 communicates with an inlet of a first vacuum pump 20.
An outlet at the bottom of the cleaning solution storage tank 1 is respectively communicated with an airflow inlet channel and an airflow outlet channel of the first cold trap device 5 through a first valve 2 and a second valve 19, in specific implementation, two outlet channels are arranged at two sides of the bottom of the cleaning solution storage tank 1, and the two outlet channels are respectively communicated with the airflow inlet channel and the airflow outlet channel of the first cold trap device 5 through the first valve 2 and the second valve 19;
the top surface is installed respectively with first sprinkler 4 and second sprinkler 17 in the first cold hydrazine device 5 both sides after first interlayer 7 cuts apart, and first sprinkler 4 and second sprinkler 17 are located the both sides of first interlayer 7, are located two spaces that first interlayer 7 cut apart respectively. Inlets of the first spraying device 4 and the second spraying device 17 are respectively communicated with an outlet at the bottom of the cleaning solution storage tank 1, and spraying outlets of the first spraying device 4 and the second spraying device 17 spray cleaning solution towards the lower space of the inner cavity of the first cold hydrazine device 5 in the first cold hydrazine device 5; in the specific implementation, two outlet flow channels are further arranged on two sides of the bottom of the cleaning solution storage tank 1, and the two outlet flow channels are respectively communicated with the first spraying device 4 and the second spraying device 17.
The first barrier 7 is one of a planar plate-like or tubular structure dividing the first inlet heating pipe 3 and the first outlet heating pipe 18 in the first cold trap device 5, and the first barrier 7 may be hollow or solid.
The second cold trap device 27 has substantially the same layout as the first cold trap device 5.
A second condensation jacket 26 is arranged on the outer wall of the upper middle part of the second cold trap device 27, and the second condensation jacket 26 is used for condensing the gaseous phenol falling to the upper middle part of the second cold trap device 27 to form a liquid state or a solid state;
the lower part of the second cold trap device 27 is provided with a second heating bottom shell 29, and the second heating bottom shell 29 is used for heating the liquid phenol or solid phenol falling to the lower part of the second cold trap device 27 to form liquid phenol;
a vertically arranged second interlayer 28 is fixedly arranged in the middle of the inner top surface between the two sides of the second cold hydrazine device 27, the upper end of the second interlayer 28 is fixedly and hermetically connected with the inner top surface of the second cold hydrazine device 27, and the lower end of the second interlayer extends downwards to the outlet at the bottom end of the second cold hydrazine device 27 and is lower than the second condensation jacket 26, so that the inner cavity of the second cold hydrazine device 27 is divided into two local inner cavities at the two sides.
The second barrier 28 is one of a planar plate-like or tubular structure dividing the second inlet heating conduit 14 and the second outlet heating conduit 24 in the second cold trap device 27, and the second barrier 28 may be hollow or solid.
An airflow inlet channel and an airflow outlet channel are arranged on the two sides of the second cold trap device 27 divided by the second partition layer 28 and extend outwards, the airflow inlet channel and the airflow outlet channel are located on the two sides of the second partition layer 28, the airflow inlet channel is used for introducing inert gas such as mixed gas of nitrogen and a small amount of gaseous phenol, the airflow outlet channel is used for flowing out the inert gas such as nitrogen, the airflow inlet channel is communicated with a second inlet heating pipeline 14 which mainly inputs the inert gas such as nitrogen, and the airflow outlet channel is communicated with a second outlet heating pipeline 24; the second outlet heating conduit 24 is in communication with the inlet of the second vacuum pump 21 via a seventh valve 25.
The top surfaces of the two sides of the second cold trap device 27 divided by the second interlayer 28 are respectively provided with a third spraying device 22 and a fourth spraying device 23, and the third spraying device 22 and the fourth spraying device 23 are positioned on the two sides of the second interlayer 28 and respectively positioned in two spaces divided by the second interlayer 28. Inlets of a third spraying device 22 and a fourth spraying device 23 are respectively communicated with an outlet at the bottom of the cleaning solution storage tank 1, and spraying outlets of the third spraying device 22 and the fourth spraying device 23 spray cleaning solution towards the lower space of the inner cavity of the second cold hydrazine device 27 in the second cold hydrazine device 27; in specific implementation, two outlet flow channels are further arranged on two sides of the bottom of the cleaning solution storage tank 1, and the two outlet flow channels are respectively communicated with the third spraying device 22 and the fourth spraying device 23.
Thus, one side of the first cold trap device 5 is connected with a first inlet heating pipeline 3 continuously inputting phenol mainly, the other side is connected with a first outlet heating pipeline 18, and the other end of the first outlet heating pipeline 18 is connected into a first vacuum system manufactured by a first vacuum pump 20.
The second cold trap device 27 is connected to a second vacuum system manufactured by a second vacuum pump 21 through a seventh valve 25 via a second outlet heating pipeline 24, and is connected to the inner wall of the phenol collecting tank 11 through an eighth valve 30 via a second heating bottom shell 29.
An outlet at the bottom end of the first cold trap device 5 is respectively communicated with an inert gas supply port 10, a phenol collecting tank 11 and a second inlet heating pipeline 14 through a four-way joint;
the middle part of the phenol collecting tank 11 is provided with a port for phenol to flow through, the port is arranged obliquely upwards and is communicated with the outlet at the bottom end of the second cold trap device 27 after passing through the eighth valve 30.
The first cold trap device 5 and the phenol collecting tank 11 are respectively connected to the upper end and the lower end of the four-way joint, and the inert gas supply port 10 and the second inlet heating pipeline 14 are respectively connected to the ports on the two horizontal sides of the four-way joint. An inert gas such as nitrogen is introduced from the inert gas supply port 10 at all times.
The outlet at the bottom end of the first cold hydrazine device 5 is connected with the four-way valve through a third valve 16, the inert gas supply port 10 is connected with the four-way valve through a fourth valve 9, the second inlet heating pipeline 14 is connected with the four-way valve through a fifth valve 15, and the phenol collecting tank 11 is directly connected with the four-way valve.
Thus, the phenol collecting tank 11 is connected to the inert gas supply port 10 through the fourth valve 9, connected to the first heating bottom shell 8 through the third valve 16, and connected to the second cold trap device 27 through the second inlet heating pipe 14 through the fifth valve 15. The fifth valve 15 is not normally opened, and only when the phenol liquid in the phenol collecting tank 11 is evacuated and the air pressure is normal pressure, the valve 15 is opened at the same time under the state that the valves 16 and 9 are closed, and the near vacuum system manufactured by the second vacuum pump 21 is utilized to change the vacuum degree in the phenol collecting tank 11 to be consistent with the vacuum degree in the first cold trap 5, so that the vacuum in the first cold trap 5 cannot be damaged when the valve 16 is opened under the condition that the valves 9, 15 and 30 are closed.
The outlet at the bottom of the phenol collecting tank 11 is communicated with a phenol discharging port 12 through a sixth valve 13, and the phenol discharging port 12 is connected to an external phenol collecting place.
In specific implementation, besides the first spraying device 4, the second spraying device 17, the third spraying device 22 and the fourth spraying device 23, a plurality of spraying devices can be additionally arranged.
The condensation temperature of the first condensation jacket 6 and the second condensation jacket 26 is-100 to 43 ℃.
The first inlet heating pipeline 3, the first outlet heating pipeline 18, the first heating bottom shell 8, the second inlet heating pipeline 14, the second outlet heating pipeline 24, the second heating bottom shell 29, the phenol collecting tank 11 and the outer wall of phenol direct contact fittings are all provided with heating fitting jackets for heating phenol to prevent phenol from solidifying, and the temperature of the heating fittings is 43-300 ℃. The heating fitting may be a heating jacket.
In the cleaning solution storage tank 1, the cleaning solution has a boiling point higher than the temperatures of the first inlet heating pipe 3, the first outlet heating pipe 18, the first heating bottom shell 8, the second inlet heating pipe 14, the second outlet heating pipe 24, the second heating bottom shell 29 and the heating fittings in the phenol collection tank 11, and a freezing point lower than the temperatures of the first condensation jacket 6 and the second condensation jacket 29.
Through the main body design of the phenol extraction device, small molecules such as phenol extracted from the system can be condensed by the first condensation jacket 6 and then liquefied by the first heating bottom shell 8 and flow into the phenol collection tank 11, and extraction of the small molecules such as phenol is completed.
In the initial state, the first valve 2, the second valve 19, the fourth valve 9, the fifth valve 15, the sixth valve 13, the seventh valve 25, and the eighth valve 30 are all closed, and the third valve 16 is opened.
When the first vacuum pump 20 is turned on to perform air extraction, mixed gas of gaseous phenol and a very small amount of oligomers enters the first cold trap device 5 from the first inlet heating pipeline 3 and the airflow inlet channel, flows into the upper middle space of the partial inner cavity of the first cold trap device 5 close to one side of the first inlet heating pipeline 3, is condensed into a liquid state or a solid state by the first condensation jacket 6 at the side, and falls into the lower space of the partial inner cavity of the first cold trap device 5 under the action of gravity;
meanwhile, the gaseous phenol can enter the upper middle space of the partial inner cavity of the first cold hydrazine device 5 close to one side of the first outlet heating pipeline 18 by winding the gaseous phenol through the first interlayer 7 under the condition that the gaseous phenol is not fully condensed by the first condensing jacket 6 close to one side of the first inlet heating pipeline 3, and the gaseous phenol is further condensed into a liquid state or a solid state by the first condensing jacket 6 on the side and falls into the lower space of the partial inner cavity of the first cold hydrazine device 5 under the action of gravity, and the gaseous phenol can be fully condensed by the first condensing jacket 6 through the air flow design of a circuitous route.
And under the condition that the first vacuum pump 20 is turned on for pumping, inert gas such as nitrogen in the mixed gas flows out to the outside from the gas flow outlet channel and the first outlet heating pipeline 18 after bypassing the first interlayer 7.
The liquid phenol and the solid phenol falling into the lower space of the partial inner cavity of the first cold trap device 5 are continuously heated by the first heating bottom shell 8 to form stable liquid phenol, and then flow into the phenol collecting tank 11 through the third valve 16 and the four-way valve.
When phenol is condensed into a solid state by the first condensation jacket 6 and is adhered to the inner wall surface and cannot fall off, or a large block of solid phenol falls off from the inner wall surface of the first condensation jacket 6 and cannot be rapidly heated and melted by the first heating bottom shell 8, or high-melting-point oligomers are accumulated in the wall surface of the pipeline, the first valve 2 and the second valve 19 are opened, so that the cleaning solution in the cleaning solution storage tank 1 flows into the two local inner cavities after flowing through the airflow inlet channel and the airflow outlet channel of the first cold hydrazine device 5, and the first spraying device 4 and the second spraying device 17 are opened, so that the cleaning solution in the cleaning solution storage tank 1 is sprayed into the two local inner cavities, and the cleaning solution flowing into the two local inner cavities can finally melt the solid phenol or the high-melting-point oligomers inside the first cold hydrazine device 5.
When the liquid (containing phenol and the washing liquid) in the phenol collection tank 11 is filled to an excess level, the third valve 16 is closed, the fourth valve 9 is opened, an inert gas such as nitrogen is introduced from the inert gas supply port 10 to make the pressure in the phenol collection tank 11 reach the normal pressure, and then the sixth valve 13 is opened to discharge the liquid in the phenol collection tank 11 from the phenol discharge port 12.
Then the fourth valve 9 and the sixth valve 13 are closed, the fifth valve 15 is opened, the inner cavities of the phenol collecting tank 11 and the second cold trap device 27 are communicated with the second inlet heating pipeline 14 through the four-way valve, and the second vacuum pump 21 is opened to perform air suction work, so that the vacuum in the phenol collecting tank 11 is consistent with the first vacuum system in the first cold trap device 5;
then, the fifth valve 15 is closed, the third valve 16 is opened, the phenol collection tank 11 is communicated with the first cold trap device 5, and phenol collected by the first cold trap device 5 is collected continuously.
After the second cold hydrazine device 27 is communicated with the phenol collecting tank 11, the local gaseous phenol flows into the inner cavity of the second cold hydrazine device 27 from the phenol collecting tank 11 through the four-way and the second inlet heating pipeline 14, and the second cold hydrazine device 27 realizes the function and the treatment process which are basically consistent with those of the first cold hydrazine device 5.
When the accumulated liquid at the bottom of the second cold trap device 27 is too much, the eighth valve 30 is opened after the liquid in the phenol collecting tank 11 is emptied, so that the accumulated liquid in the second heating bottom shell 29 flows into the phenol collecting tank 11, and the third spraying device 22 and the fourth spraying device 23 can be opened for cleaning.
Thus, by the above pipe connection design, when the third valve 16 is opened, the first cold trap device 5 and the phenol collection tank 11 are in the first vacuum system, and the fifth valve 15 and the eighth valve 30 are closed and isolated from the second vacuum system in which the second cold trap device 27 is located, phenol and oligomers condensed by the first cold trap device 5 are continuously collected into the phenol collection tank 11, when the phenol liquid level in the phenol collection tank 11 is at a position of 1/5 to 4/5 of the tank body, the third valve 16 is closed, the phenol collection tank 11 is separated from the first vacuum system, the fourth valve 9 is communicated with the inert gas supply port 10, inert gas such as nitrogen is filled to make the phenol collection tank 11 form normal pressure, the sixth valve 13 is opened to discharge small molecules such as phenol in the tank, the fourth valve 9 and the sixth valve 13 are closed, the fifth valve 15 is opened to connect to the second vacuum system, the vacuum in the phenol collection tank 11 is made to be consistent with the first vacuum system, then the fifth valve 15 is closed, the third valve 16 is opened, and the phenol collection tank 11 is continuously collected from the phenol collection system through the small molecule vacuum system.
The design of the phenol collecting tank 11 can ensure that small molecules such as phenol are smoothly discharged, and the second vacuum system is introduced to adjust the vacuum in the phenol collecting tank 11 after the small molecules such as phenol are discharged to be consistent with the first vacuum system, so that the fluctuation interference to the first vacuum system when the third valve 16 is opened is avoided. The establishment of second cold hydrazine device 27 can protect second vacuum pump 21 not corroded by phenol, can open eighth valve 30 after the evacuation of liquid in phenol collection tank 11 when second cold hydrazine device 27 bottom hydrops is too much, makes in the second heating drain pan 29 hydrops flow into phenol collection tank 11.
The design can be convenient for cleaning the pipeline in real time in the production process, and small molecules such as phenol, oligomers and the like are prevented from blocking the pipeline.
The controllable cleaning device can effectively prevent phenol, oligomer and the like from forming large blocks at the cold hydrazine position to be accumulated, the cleaning process can be carried out in the continuous production process, and the establishment of the controllable cleaning device provides guarantee for the long-term operation of the device.
The design can fully condense the small molecules such as phenol and the like, and the extraction is complete.
The device can continuously extract phenol, and meanwhile, the device can be effectively cleaned under the condition of no stopping, so that devices are prevented from being damaged, and the long-term operation of a vacuum system is ensured.
Preferably, the temperature of all the heating zones of the first inlet heating pipeline 3, the first outlet heating pipeline 18, the first heating bottom shell 8, the second inlet heating pipeline 14, the second outlet heating pipeline 24, the second heating bottom shell, the phenol collecting tank 11 and the like is above 43 ℃. The temperature of the first condensation jacket 6 and the second condensation jacket 26 is between-10 ℃ and 0 ℃, the low temperature maintenance of the condensation jackets depends on external low-temperature constant-temperature circulation equipment, and the circulation medium adopts sodium chloride aqueous solution with certain concentration.
Preferably, the small molecules such as phenol in the apparatus can be washed using ethylene glycol, diethylene glycol, or n-propanol as a washing liquid.
Preferably, the phenol extraction apparatus shown in FIG. 1 can be used in series with 1 to 3 apparatuses.
The above description is only an embodiment of the present invention, but the structural features of the present invention are not limited thereto, and any changes or modifications within the scope of the present invention by those skilled in the art are covered by the present invention.
Claims (9)
1. The utility model provides a can move phenol extraction element for a long time which characterized in that:
the device comprises a cleaning solution storage tank (1), a first cold trap device (5), a phenol collection tank (11) and a second cold trap device (27), wherein the cleaning solution storage tank (1) is positioned above the side of the first cold trap device (5), and the second cold trap device (27) is arranged on the side of the phenol collection tank (11); the bottom of the cleaning solution storage tank (1) is communicated with a first cold trap device (5), the bottom of the first cold trap device (5) is respectively communicated with a phenol collection tank (11), and the phenol collection tank (11) is communicated with a second cold trap device (27).
2. The long-term operable phenol recovery apparatus of claim 1, wherein:
in the first cold trap device (5): the outer wall of the upper middle part of the first cold hydrazine device (5) is provided with a first condensation jacket (6), and the first condensation jacket (6) is used for condensing the gaseous phenol falling to the upper middle part of the first cold hydrazine device (5) to form a liquid state or a solid state; the lower part of the first cold trap device (5) is provided with a first heating bottom shell (8), and the first heating bottom shell (8) is used for heating liquid phenol or solid phenol falling to the lower part of the first cold trap device (5) to form liquid phenol; a vertically arranged first interlayer (7) is fixedly arranged in the middle of the inner top surface between the two sides of the first cold hydrazine device (5), the upper end of the first interlayer (7) is fixedly and hermetically connected with the inner top surface of the first cold hydrazine device (5), and the lower end of the first interlayer extends downwards to the outlet at the bottom end of the first cold hydrazine device (5), so that the inner cavity of the first cold hydrazine device (5) is divided into two local inner cavities at the two sides;
in the second cold trap device (27): a second condensation jacket (26) is arranged on the outer wall of the upper middle part of the second cold trap device (27), and the second condensation jacket (26) is used for condensing the gaseous phenol falling to the upper middle part of the second cold trap device (27) to form a liquid state or a solid state; the lower part of the second cold trap device (27) is provided with a second heating bottom shell (29), and the second heating bottom shell (29) is used for heating liquid phenol or solid phenol falling to the lower part of the second cold trap device (27) to form liquid phenol; the middle of the inner top surface between the two sides of the second cold trap device (27) is fixedly provided with a vertically arranged second interlayer (28), the upper end of the second interlayer (28) is fixedly and hermetically connected with the inner top surface of the second cold trap device (27), and the lower end of the second interlayer extends downwards to the outlet at the bottom end of the second cold trap device (27), so that the inner cavity of the second cold trap device (27) is divided into two local inner cavities at the two sides.
3. The phenol extraction plant of claim 1, wherein:
in the first cold trap device (5): an airflow inlet channel and an airflow outlet channel extend upwards from two sides of the first cold trap device (5) divided by the first interlayer (7), the airflow inlet channel is communicated with a first inlet heating pipeline (3) which is mainly continuously input with gaseous phenol, and the airflow outlet channel is communicated with a first outlet heating pipeline (18); the first outlet heating pipeline (18) is communicated with an inlet of a first vacuum pump (20); an outlet at the bottom of the cleaning solution storage tank (1) is respectively communicated with an airflow inlet channel and an airflow outlet channel of the first cold trap device (5) through a first valve (2) and a second valve (19); the inner top surfaces of two sides of the first cold hydrazine device (5) after the first interlayer (7) is divided are respectively provided with a first spraying device (4) and a second spraying device (17), and inlets of the first spraying device (4) and the second spraying device (17) are respectively communicated with an outlet at the bottom of the cleaning solution storage tank (1);
in the second cold trap device (27): an airflow inlet channel and an airflow outlet channel extend outwards from two sides of the second cold trap device (27) divided by the second interlayer (28), the airflow inlet channel is communicated with a second inlet heating pipeline (14) for mainly inputting inert gas, and the airflow outlet channel is communicated with a second outlet heating pipeline (24); the second outlet heating pipeline (24) is communicated with the inlet of the second vacuum pump (21) through a seventh valve (25); and the top surfaces of the two sides of the second cold trap device (27) divided by the second interlayer (28) are respectively provided with a third spraying device (22) and a fourth spraying device (23), and inlets of the third spraying device (22) and the fourth spraying device (23) are respectively communicated with an outlet at the bottom of the cleaning solution storage tank (1).
4. The long-term operable phenol recovery apparatus of claim 1, wherein:
an outlet at the bottom end of the first cold trap device (5) is respectively communicated with an inert gas supply port (10), a phenol collecting tank (11) and a second inlet heating pipeline (14) through a four-way joint;
and a port for phenol circulation is arranged in the middle of the phenol collecting tank (11), is obliquely and upwards arranged and is communicated with an outlet at the bottom end of the second cold hydrazine device (27) after passing through an eighth valve (30).
5. The phenol extraction plant of claim 4, wherein:
the first cold hydrazine device (5) and the phenol collecting tank (11) are respectively connected to the upper end and the lower end of the cross joint, and the inert gas supply port (10) and the second inlet heating pipeline (14) are respectively connected to the ports on the two horizontal sides of the cross joint.
6. The long-term-operable phenol recovery plant of claim 4, wherein:
the outlet at the bottom end of the first cold hydrazine device (5) is connected with the four-way valve through a third valve (16), the inert gas supply port (10) is connected with the four-way valve through a fourth valve (9), the second inlet heating pipeline (14) is connected with the four-way valve through a fifth valve (15), and the phenol collecting tank (11) is directly connected with the four-way valve.
7. The phenol extraction plant of claim 4, wherein:
and an outlet at the bottom of the phenol collecting tank (11) is communicated with a phenol discharge port (12) through a sixth valve (13).
8. The phenol extraction plant of claim 1, wherein:
the first inlet heating pipeline (3), the first outlet heating pipeline (18), the first heating bottom shell (8), the second inlet heating pipeline (14), the second outlet heating pipeline (24), the second heating bottom shell (29), the phenol collecting tank (11) and the outer wall of the phenol direct contact fitting are provided with heating fitting clamping sleeves.
9. The phenol extraction plant of claim 1, wherein:
in the cleaning solution storage tank (1), the boiling point of the cleaning solution is higher than the temperatures of a first inlet heating pipeline (3), a first outlet heating pipeline (18), a first heating bottom shell (8), a second inlet heating pipeline (14), a second outlet heating pipeline (24), a second heating bottom shell (29) and heating accessories in the phenol collection tank (11), and the freezing point is lower than the temperatures of the first condensation jacket (6) and the second condensation jacket (29).
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| CN202111562021.9A CN115245789B (en) | 2021-12-17 | 2021-12-17 | Phenol extraction device capable of long-term operation |
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| CN202111562021.9A CN115245789B (en) | 2021-12-17 | 2021-12-17 | Phenol extraction device capable of long-term operation |
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| CN110538481A (en) * | 2019-10-11 | 2019-12-06 | 中国科学院过程工程研究所 | Phenol continuous extraction system, polycarbonate resin production system comprising phenol continuous extraction system and production method |
| CN213467305U (en) * | 2020-10-19 | 2021-06-18 | 山东建筑大学 | Energy-saving device for efficiently recycling phenol waste gas |
| CN214598057U (en) * | 2020-11-27 | 2021-11-05 | 海南华盛新材料科技有限公司 | Be used for producing polycarbonate tail gas processing apparatus |
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| CN101104585A (en) * | 2007-06-01 | 2008-01-16 | 郑金星 | Device for producing methyl methacrylate by using waste and old organic glass and using method thereof |
| WO2019049027A1 (en) * | 2017-09-06 | 2019-03-14 | Sabic Global Technologies B.V. | A method of recovering phenol in a melt polycarbonate polymerization |
| CN209679540U (en) * | 2019-01-31 | 2019-11-26 | 河北诚信集团有限公司 | Cyanuric Chloride liquefying plant |
| CN110538481A (en) * | 2019-10-11 | 2019-12-06 | 中国科学院过程工程研究所 | Phenol continuous extraction system, polycarbonate resin production system comprising phenol continuous extraction system and production method |
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