CN119220994A - A production device and method for perfluorotributylamine capable of deep fluorination - Google Patents
A production device and method for perfluorotributylamine capable of deep fluorination Download PDFInfo
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- CN119220994A CN119220994A CN202411758327.5A CN202411758327A CN119220994A CN 119220994 A CN119220994 A CN 119220994A CN 202411758327 A CN202411758327 A CN 202411758327A CN 119220994 A CN119220994 A CN 119220994A
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- heat exchange
- pipe
- tank body
- electrolytic cell
- perfluorotributylamine
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- RVZRBWKZFJCCIB-UHFFFAOYSA-N perfluorotributylamine Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)N(C(F)(F)C(F)(F)C(F)(F)C(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F RVZRBWKZFJCCIB-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 238000003682 fluorination reaction Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title description 13
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 210000005056 cell body Anatomy 0.000 claims abstract description 18
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 9
- 239000003507 refrigerant Substances 0.000 claims description 44
- 238000004140 cleaning Methods 0.000 claims description 34
- 230000005540 biological transmission Effects 0.000 claims description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 claims description 25
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 230000007246 mechanism Effects 0.000 claims description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 7
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 7
- 230000000712 assembly Effects 0.000 claims description 4
- 238000000429 assembly Methods 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 239000003792 electrolyte Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000006073 displacement reaction Methods 0.000 claims 2
- 210000004027 cell Anatomy 0.000 claims 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 1
- 239000012530 fluid Substances 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 7
- 238000009825 accumulation Methods 0.000 abstract description 6
- 239000013049 sediment Substances 0.000 abstract description 6
- 238000013461 design Methods 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- 238000004891 communication Methods 0.000 description 14
- 239000000047 product Substances 0.000 description 14
- 230000006872 improvement Effects 0.000 description 9
- 230000008569 process Effects 0.000 description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000012452 mother liquor Substances 0.000 description 5
- 230000000149 penetrating effect Effects 0.000 description 4
- -1 perfluoro tertiary amine compound Chemical class 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- 101100298048 Mus musculus Pmp22 gene Proteins 0.000 description 1
- UGAPHEBNTGUMBB-UHFFFAOYSA-N acetic acid;ethyl acetate Chemical compound CC(O)=O.CCOC(C)=O UGAPHEBNTGUMBB-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000002473 artificial blood Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 210000002381 plasma Anatomy 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B15/00—Operating or servicing cells
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B15/00—Operating or servicing cells
- C25B15/02—Process control or regulation
- C25B15/021—Process control or regulation of heating or cooling
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B3/00—Electrolytic production of organic compounds
- C25B3/01—Products
- C25B3/09—Nitrogen containing compounds
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B3/00—Electrolytic production of organic compounds
- C25B3/01—Products
- C25B3/11—Halogen containing compounds
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B3/00—Electrolytic production of organic compounds
- C25B3/20—Processes
- C25B3/27—Halogenation
- C25B3/28—Fluorination
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
- C25B9/60—Constructional parts of cells
- C25B9/67—Heating or cooling means
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Automation & Control Theory (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
本发明涉及全氟三丁胺制备技术领域，尤其涉及一种能深度氟化的全氟三丁胺生产装置及其生产方法，其结构包括：电解槽本体，电解槽本体的一侧向外设置有母液进液管，以及用于对电解槽本体内物料进行循环制冷的换热装置，本发明将多管路换热管更替为单一管路式，流动路径较为简单，流体在同一管道中流动，流速较为均匀，避免了多管路设计中因流量分布不均而导致的某些管道流速过慢，造成局部淤积的现象，同时采用螺旋向下延伸设置，使产品沿着管道的曲线流动，增加流体的扰动和湍流度，这种扰动流动有助于防止电解产物沉积在管道内壁，因为湍流能够提高流体的剪切力，有效地冲刷掉沉积物，避免了物质在管道内积累，并有效保证换热均匀和效率。
The invention relates to the technical field of perfluorotributylamine preparation, and in particular to a perfluorotributylamine production device capable of deep fluorination and a production method thereof. The structure comprises: an electrolytic cell body, a mother liquid inlet pipe is arranged outwardly on one side of the electrolytic cell body, and a heat exchange device for circulating and refrigerating materials in the electrolytic cell body. The invention replaces a multi-pipeline heat exchange tube with a single-pipeline type, the flow path is relatively simple, the fluid flows in the same pipeline, the flow velocity is relatively uniform, and the phenomenon of slow flow velocity in some pipelines due to uneven flow distribution in the multi-pipeline design is avoided, resulting in local silting. At the same time, a spiral downward extension is adopted to make the product flow along the curve of the pipeline, thereby increasing the disturbance and turbulence of the fluid. The disturbed flow helps to prevent the electrolysis product from being deposited on the inner wall of the pipeline, because the turbulence can increase the shear force of the fluid, effectively wash away the sediment, avoid the accumulation of substances in the pipeline, and effectively ensure the uniformity and efficiency of heat exchange.
Description
Technical Field
The invention relates to the technical field of preparation of perfluorotributylamine, in particular to a perfluorotributylamine production device capable of deeply fluorinating and a production method thereof.
Background
The perfluoro tributylamine molecule is an important perfluoro tertiary amine compound, and has wide application in modern civilization society due to the excellent physical, chemical and physiological properties. The perfluoro tributylamine is colorless transparent liquid at normal temperature, has almost no smell of amine, is insoluble in water and ethanol, has very small solubility in butanone, diethyl ether, chloroform, dioxane, acetic acid ethyl acetate, benzene, petroleum ether and other organic solvents, and can be mixed with fluorochloroalkane. The perfluoro tributylamine is completely nontoxic to human body, can dissolve and carry a large amount of oxygen and carbon dioxide, and is one of the main components of artificial blood plasma applied in the modern medical field. Simultaneously used as an anti-corrosion transmission liquid and a dielectric insulating liquid of instruments and meters, leak detection liquid for electronic elements and devices. The production of perfluoro tributylamine has great significance for national science progress and development.
The prior art for preparing the perfluorinated tributylamine has the most widely applied method, namely, a mother solution consisting of the tributylamine and hydrogen fluoride is introduced into an electrolytic tank by adopting an electrolytic fluorination method, low-voltage direct current is introduced into the electrolytic tank to generate free fluorine atoms to directly replace hydrogen atoms in the tributylamine, and then the perfluorinated tributylamine product is obtained through simple purification treatment. The electrolysis process belongs to an exothermic state, mother liquor and products are required to be cooled in a circulating way through corresponding refrigeration heat exchangers, so that the problem that materials are gasified due to temperature rise in the electrolysis process is solved, the defects that the existing heat exchange pipeline adopts a multi-pipeline simultaneous heat exchange mode, so that the electrolytic products are easy to pool, in the heat exchange process, refrigerants are generally injected from the top of a heat exchange tank to flow downwards directly, in the heat exchange tank, the refrigerants possibly flow faster along certain channels, flow rates in other areas are slower, dead zones exist in the heat exchange process, due to uneven flow rates, the contact time of part of refrigerants possibly flowing through the heat exchange pipe is shorter, the heat of pipe walls cannot be fully absorbed, the cooling effect is poor, and the heat exchange efficiency is low;
The heat exchanger has the great problem that along with the increase of the service time, scaling substances (such as scale, rust and the like) and other sediments in the refrigerant can accumulate on the pipe wall of the heat exchanger, so that the heat exchange and electrolysis reaction efficiency is reduced, even equipment is damaged, and if the heat exchange pipe of the heat exchanger is removed and cleaned, the electrolytic tank is required to be stopped, and the production process is also influenced.
Disclosure of Invention
The invention provides a device and a method for producing perfluorotributylamine capable of deeply fluorinating, which can effectively solve the problems.
The invention is realized in the following way:
The perfluorinated tributyl amine production device capable of deeply fluorinating comprises an electrolytic tank body, wherein one side of the electrolytic tank body is outwards provided with a mother liquor inlet pipe and a heat exchange device for circularly refrigerating materials in the electrolytic tank body, the heat exchange device comprises a heat exchange tank body, a circulating liquid guide pipe is arranged in the heat exchange tank body, one end of the circulating liquid guide pipe is connected to the top of the heat exchange tank body in a penetrating manner and is pumped to the bottom of the electrolytic tank body through a circulating feeding pipe, the other end of the circulating liquid guide pipe is connected to the bottom of the heat exchange tank body in a penetrating manner and is connected to the top of the bottom of the electrolytic tank body through a circulating discharging pipe, the circulating feeding pipe is outwards connected with a product discharging pipe through a three-way valve, and a densimeter for detecting the density of the materials is arranged at the bottom of the electrolytic tank body; the circulating liquid guide pipe comprises an input pipe connected to the top of the heat exchange tank body, an output pipe connected to the bottom of the heat exchange tank body, and a heat exchange flow pipe which is positioned in the heat exchange tank body and is connected between the input pipe and the output pipe, wherein the heat exchange flow pipe extends downwards in a spiral manner, a refrigerant feeding pipe is arranged at the top of the left side of the heat exchange tank body, a refrigerant discharging pipe is arranged at the bottom of the right side of the heat exchange tank body, a plurality of groups of flow guiding devices communicated with the heat exchange tank body are respectively arranged at two sides of the heat exchange tank body, each group of flow guiding devices comprises a flow inlet device and a flow outlet device, a feeding pump arranged between the flow inlet device and the flow outlet device, the inlet end of the flow inlet device is communicated with the heat exchange tank body, the outlet end of the flow outlet device is connected with the feeding port of the feeding pump, the flow inlet device of the uppermost flow guiding device on the right side is correspondingly arranged with the refrigerant feeding pipe, the flow outlet device on the right side is correspondingly arranged with the flow inlet device of the flow guiding device on the left side, the heat exchange device comprises a heat exchange tank body, a left side flow guiding device, a right side flow guiding device, a cleaning mechanism and a cleaning mechanism, wherein the flow inlet of the left side flow guiding device is correspondingly arranged with the flow outlet of the right side flow guiding device, the flow outlet of the left side lowest flow guiding device is correspondingly arranged with the refrigerant discharge pipe, the cleaning mechanism is arranged in the heat exchange tank body, and when a refrigerant enters the heat exchange tank body through a refrigerant feeding pipe to cool the heat exchange flow pipe, the cleaning mechanism moves up and down circularly along the heat exchange flow pipe for cleaning.
As a further improvement, the flow inlet device and the flow outlet device comprise a box body, the box body is provided with a first communication port connected with the heat exchange tank body, the box body is provided with a second communication port connected with the feeding pump, a plurality of flow dividing plates extending from the first communication port to the second communication port are arranged in the box body, and the first communication port is provided with a filter screen.
As a further improvement, the cleaning mechanism comprises a rotating shaft coaxially arranged with the heat exchange runner pipe, a connecting cylinder is sleeved on the surface of the rotating shaft, a transmission screw rod sleeved in the rotating shaft is fixed in the heat exchange tank body, a track corresponding to the spiral of the heat exchange runner pipe is arranged on the transmission screw rod, a guide rail extending vertically is arranged on the rotating shaft, a guide post matched with the guide rail and the transmission screw rod track is arranged on the inner side of the connecting cylinder, the connecting cylinder is externally connected with a lantern ring through a connecting rod, the lantern ring is correspondingly sleeved on the outer side of the heat exchange runner pipe, a cleaning brush is arranged in the lantern ring, a speed reducing motor is arranged at the top of the heat exchange tank body, and an output shaft of the speed reducing motor is fixedly connected with the rotating shaft.
As a further improvement, the cleaning brush comprises an annular frame coaxially arranged in the lantern ring, a plurality of brush head assemblies are uniformly distributed on the inner side of the annular frame, a positioning plate which extends outwards is arranged on one side of the annular frame, first transmission teeth are uniformly distributed on the inner side of the positioning plate, a transmission rod is sleeved on the connecting rod, second transmission teeth are arranged on one side of the guide rail, a first gear meshed with the first transmission teeth is arranged at one end of the transmission rod, and a second gear meshed with the second transmission teeth is arranged at the other end of the transmission rod.
As a further improvement, the brush head assembly comprises a driving shaft which is annularly distributed on the annular frame, one end of the driving shaft facing the inner side of the annular frame is fixedly provided with a brush head, the other end of the driving shaft is fixedly provided with a third gear, and the lantern ring is provided with a third transmission tooth matched with the third gear.
As a further improvement, the electrolytic tank body is internally provided with anode plates and cathode plates for electrolytic reaction, the anode plates and the cathode plates are vertically and alternately arranged, the top of the electrolytic tank body is provided with a circulating liquid uniform distributor connected with a circulating discharge pipe, and the bottom of the circulating liquid uniform distributor is provided with a plurality of circulating liquid discharge ports.
As a further improvement, the product discharge pipes are connected to respective intermediate tanks which are pumped to the feed end of the distillation apparatus.
As a further improvement, the top of the electrolytic tank body is connected with a tail gas discharge pipe.
As a further improvement, the left side of the electrolytic tank body is connected with a nitrogen replacement pipe, and the nitrogen replacement pipe is connected to an external nitrogen source.
A production method of perfluorinated tributyl amine comprises the following specific steps of S, replacing air in an electrolytic tank body by nitrogen before reaction, preliminarily mixing the air with the nitrogen to prepare electrolyte in the electrolytic tank body, S2, respectively preparing tributyl amine and hydrogen fluoride according to the mass ratio of 24-30 kg to 200-230 kg, firstly adding hydrogen fluoride into the electrolytic tank body, then adding tributyl amine, S3, introducing low-voltage current to perform electrolytic replacement reaction, controlling the reaction pressure of the electrolytic tank to be 0.1-1.5 MP and the temperature to be 5-15 ℃, S5, after the electrolysis is completed, carrying out electrolytic fluorination on the tributyl amine to convert the tributyl amine into perfluorinated tributyl amine, and discharging the perfluorinated tributyl amine from the bottom of the electrolytic tank body to obtain the perfluorinated tributyl amine.
The beneficial effects of the invention are as follows:
The invention replaces the multi-pipeline heat exchange tube into a single pipeline type, the flow path is simpler, the fluid flows in the same pipeline, the flow speed is more uniform, the phenomenon of local siltation caused by too slow flow speed of certain pipelines due to uneven flow distribution in the design of the multi-pipeline is avoided, meanwhile, the spiral downward extension arrangement is adopted, the product flows along the curve of the pipeline, the disturbance and the turbulence of the fluid are increased, the disturbance flow is helpful to prevent the electrolytic product from being deposited on the inner wall of the pipeline, and the turbulence can improve the shearing force of the fluid, effectively wash away the sediment, avoid the accumulation of substances in the pipeline, and effectively ensure the uniformity and the efficiency of heat exchange. According to the invention, the flow guiding device is arranged, so that the flow direction of the refrigerant in the heat exchange tank body is changed by adopting a baffling flow mode, the refrigerant is caused to repeatedly contact with the surface of the heat exchange flow pipe for a plurality of times, the residence time of the refrigerant in the heat exchanger is increased, thereby more time is allowed to exchange heat with the heat exchange surface, the heat exchange efficiency is further improved, the refrigerant is prevented from flowing unevenly, and the refrigerant is ensured to uniformly flow through the heat exchange pipe in the heat exchanger. The invention can remove structural substances (such as dirt, grease, scale and the like) accumulated on the surface of the heat flow pipe in the refrigerant under the condition of no shutdown by arranging the cleaning mechanism, thereby ensuring the heat exchange efficiency.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a device for producing perfluorotributylamine capable of deep fluorination;
FIG. 2 is a schematic view of a heat exchange device according to the present invention;
FIG. 3 is a schematic view of a heat exchange device according to the present invention;
FIG. 4 is a schematic view of a heat exchange device according to the present invention in a front cross-sectional configuration;
FIG. 5 is a schematic diagram of a cross-sectional structure of the inlet and the outlet in a top view;
FIG. 6 is a schematic view of a cleaning mechanism according to the present invention;
FIG. 7 is a schematic view of a cleaning mechanism according to the present invention;
FIG. 8 is a schematic cross-sectional view of a connecting cylinder, connecting rod and collar provided by the invention;
FIG. 9 is a schematic cross-sectional view of a connecting cylinder, connecting rod and collar provided by the invention;
FIG. 10 is a schematic view of a structure of a cleaning brush provided by the present invention;
FIG. 11 is a schematic view in partial cross-section of a cleaning mechanism provided by the present invention;
fig. 12 is a schematic view of the structure of the electrolytic cell body provided by the invention.
In the figure, an electrolytic tank body-1, a mother liquor inlet pipe-2, a heat exchange device-3, a heat exchange tank body-31, a circulating liquor guide pipe-32, a circulating inlet pipe-4, a circulating outlet pipe-5, a three-way valve-6, a product outlet pipe-7, a densitometer-8, an input pipe-321, an output pipe-322, a heat exchange flow pipe-323, a refrigerant inlet pipe-33, a refrigerant outlet pipe-34, a flow guiding device-35, a flow inlet device-351, a flow draining device-352, a feeding pump-353, a cleaning mechanism-9, a tank body-354, a first connecting port-355, a second connecting port-356, a flow dividing plate-357, a filter screen-358, a rotating shaft-91, a connecting cylinder-92, a transmission screw-93, a guide rail-94, a guide pillar-95, a connecting rod-96, a lantern ring-97, a cleaning brush-98, a speed reducing motor-99, an annular frame-981, a brush head assembly-982, a positioning plate-983, a first transmission tooth-984, a transmission rod-985, a second transmission tooth-986, a first gear-987, a second gear-21, a third gear-21, a driving shaft-23, a third gear-102, a third gear 984, a third gear 982, a third gear 984, a circulating outlet 9810-3, a third gear 982, a circulating outlet 9810-positive plate-11, a circulating outlet 983, a circulating tank-3, a circulating outlet 983, a circulating exhaust gas-3, a circulating tank-3, a circulating exhaust tank-and a circulating-tank-and circulating tank.
Detailed Description
For the purpose of making embodiments of the present invention fall within the scope of the present invention. Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as referring to purposes, technical solutions and advantages of the present invention in any way. All other implementations, which can be derived by a person skilled in the art without making any inventive effort, show or imply relative importance or implicitly indicate the number of technical features indicated on the basis of the implementations in the invention. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
The mode that current heat exchange pipeline adopted the multitube way to exchange heat simultaneously leads to electrolysis product siltation easily to refrigerant is injected into direct downward flow by the heat exchange tank top during heat transfer generally, inside the heat exchange tank, refrigerant can flow faster along certain passageway, and flow rate is slower in other regions, there is the dead zone in the heat exchange process, because the velocity of flow is uneven, partial refrigerant can be shorter with the contact time of heat exchange tube when flowing through the heat exchange tube, can not fully absorb the heat of pipe wall, lead to the cooling effect not good, and heat exchange efficiency is low, in order to solve foretell technical problem, the proposal has proposed following technical scheme:
Referring to fig. 1-12, a deep fluorinated perfluorotributylamine production device structurally comprises an electrolytic tank body 1, a mother liquor inlet pipe 2 and a heat exchange device 3, wherein one side of the electrolytic tank body 1 is outwards provided with a mother liquor inlet pipe 2, and the heat exchange device 3 is used for circularly refrigerating materials in the electrolytic tank body 1, the heat exchange device 3 comprises a heat exchange tank body 31, a circulating liquid guide pipe 32 is arranged in the heat exchange tank body 31, one end of the circulating liquid guide pipe 32 is connected to the top of the heat exchange tank body 31 in a penetrating way and is pumped to the bottom of the electrolytic tank body 1 through a circulating inlet pipe 4, the other end of the circulating liquid guide pipe is connected to the bottom of the heat exchange tank body 31 in a penetrating way and is connected to the bottom of the electrolytic tank body 1 through a circulating outlet pipe 5, the circulating inlet pipe 4 is outwards connected with a product outlet pipe 7 through a three-way valve 6, and the bottom of the electrolytic tank body 1 is provided with a densimeter 8 for detecting the material density;
The invention replaces the multi-pipeline heat exchange tube into a single pipeline type, the flow path is simpler, the fluid flows in the same pipeline, the flow speed is more uniform, the phenomenon of local siltation caused by too slow flow speed of certain pipelines due to uneven flow distribution in the design of the multi-pipeline is avoided, meanwhile, the spiral downward extension arrangement is adopted, the product flows along the curve of the pipeline, the disturbance and the turbulence of the fluid are increased, the disturbance flow is helpful to prevent the electrolytic product from being deposited on the inner wall of the pipeline, and the turbulence can improve the shearing force of the fluid, effectively wash away the sediment, avoid the accumulation of substances in the pipeline, and effectively ensure the uniformity and the efficiency of heat exchange. The two sides of the heat exchange tank 31 are respectively provided with a plurality of groups of flow guiding devices 35 communicated with the inside of the heat exchange tank 31, each group of flow guiding devices 35 comprises a flow inlet 351 and a flow outlet 352, and a feed pump 353 arranged between the flow inlet 351 and the flow outlet 352, the inlet end of the flow inlet 351 is communicated with the inside of the heat exchange tank 31, the outlet end of the flow outlet 351 is connected with the feed inlet of the feed pump 353, the inlet end of the flow outlet 352 is communicated with the inside of the heat exchange tank 31, the flow inlet 351 of the uppermost flow guiding device 35 on the right side is correspondingly arranged with the refrigerant feed pipe 33, the flow inlet 352 of the flow guiding device 35 on the left side is correspondingly arranged with the flow outlet 352 of the flow guiding device 35 on the right side, and the flow outlet 352 of the flow guiding device 35 on the lowest left side is correspondingly arranged with the refrigerant discharge pipe 34;
As shown in fig. 4, when in use, the refrigerant enters the heat exchange tank 31 through the refrigerant feed pipe 33, flows towards the inlet 351 of the right flow guiding device 35, is conveyed towards the outlet 352 by the feed pump 353, finally returns to the heat exchange tank 31, flows towards the inlet 351 of the left flow guiding device 35, is conveyed towards the outlet 352 by the feed pump 353 of the left flow guiding device 35, returns to the heat exchange tank 31 again, circulates in sequence, and is discharged outwards through the refrigerant discharge pipe 34 until the lowest outlet 352 on the left is discharged, so that the refrigerant flows in the heat exchange tank 31 in a baffling way, the flowing direction of the refrigerant is changed, the refrigerant is promoted to repeatedly contact with the surface of the heat exchange runner pipe 323, the residence time of the refrigerant in the heat exchanger is prolonged, the heat exchange efficiency of the refrigerant and the heat exchange surface is further improved, the refrigerant is prevented from flowing unevenly, and the refrigerant is ensured to uniformly flow through the heat exchange pipe in the heat exchanger.
Wherein, the inlet 351 and the outlet 352 comprise a box 354, the box 354 is provided with a first communication port 355 connected with the heat exchange tank 31, the box 354 is provided with a second communication port 356 connected with the feed pump 353, a plurality of flow dividing plates 357 extending from the first communication port 355 to the second communication port 356 are arranged in the box 354, the first communication port 355 is provided with a filter screen 358, when in use, the refrigerant of the inlet 351 enters the box 354 from the heat exchange tank 31 through the first communication port 355 and rapidly flows to the second communication port 356 through the channels of the flow dividing plates 357, so as to enter the feed pump 353 and be conveyed to the outlet 352, and the refrigerant of the outlet 352 is conveyed to the second communication port 356 through the feed pump 353 and rapidly returns to the heat exchange tank 31 towards the first communication port 355 through the channels of the flow dividing plates 357. In order to ensure the cleanness of the surface of the heat exchange runner pipe 323 and prevent structural substances (such as dirt, grease, scaling and the like) in the refrigerant from accumulating on the surface of the heat exchange runner pipe 323, the heat exchange runner pipe 323 heat exchanger further comprises a cleaning mechanism 9 for cleaning the surface of the heat exchange runner pipe 323, wherein the cleaning mechanism 9 is arranged in the heat exchange tank 31, and when the refrigerant enters the heat exchange tank 31 through the refrigerant feeding pipe 33 to cool the heat exchange runner pipe 323, the cleaning mechanism 9 moves circularly up and down along the heat exchange runner pipe 323 to clean, thereby ensuring that the heat exchange efficiency is not affected and avoiding the reduction of the heat transfer efficiency or the equipment failure caused by the accumulation of sediments.
The cleaning mechanism 9 comprises a rotating shaft 91 coaxially arranged with a heat exchange runner pipe 323, a connecting cylinder 92 is sleeved on the surface of the rotating shaft 91, a transmission screw rod 93 sleeved in the rotating shaft 91 is fixedly arranged in the heat exchange tank 31, a track corresponding to the spiral of the heat exchange runner pipe 323 is arranged on the transmission screw rod 93, a vertically extending guide rail 94 is arranged on the rotating shaft 91, a guide pillar 95 matched with the guide rail 94 and the transmission screw rod 93 is arranged on the inner side of the connecting cylinder 92, a lantern ring 97 is connected to the outer side of the connecting cylinder 92 through a connecting rod 96, the lantern ring 97 is correspondingly sleeved on the outer side of the heat exchange runner pipe 323, a cleaning brush 98 is arranged in the lantern ring 97, a speed reducing motor 99 is arranged at the top of the heat exchange tank 31, and an output shaft of the speed reducing motor 99 is fixedly connected with the rotating shaft 91;
Therefore, when in use, the gear motor 99 drives the rotating shaft 91 to rotate in the heat exchange tank 31, meanwhile, as the connecting cylinder 92 is slidably connected to the rotating shaft 91, and the guide posts 95 on the connecting cylinder 92 are respectively in track fit with the guide rails 94 and the transmission screw rods 93, when the rotating shaft 91 rotates, the connecting cylinder 92 is driven to move up and down along the spiral of the heat exchange flow pipe 323, the connecting cylinder 92 drives the cleaning brush 98 on the collar 97 through the connecting rod 96 to remove impurities such as dirt, oil stains and sediments deposited on the surface of the heat exchange flow pipe 323, so that the accumulation of the impurities on the surface of a pipeline is avoided, the heat exchange effect is influenced, and the reduction of the heat exchange efficiency caused by the accumulation of the dirt is avoided.
Further, the cleaning brush 98 includes a ring frame 981 coaxially installed in the collar 97, a plurality of brush head assemblies 982 are uniformly distributed on the inner side of the ring frame 981, a positioning plate 983 extending outwards is disposed on one side of the ring frame 981, a first driving gear 984 is uniformly distributed on the inner side of the positioning plate 983, a driving rod 985 is sleeved on the connecting rod 96, a second driving gear 986 is disposed on one side of the guide rail 94, a first gear 987 meshed with the first driving gear 984 is disposed at one end of the driving rod 985, and a second gear 988 meshed with the second driving gear 986 is disposed at the other end of the driving rod 985, so that when the connecting cylinder 92 moves up and down along the rotation shaft 91, the second gear 988 cooperates with the second driving gear 986, thereby driving the driving rod 985 and the first gear 987 to rotate, thereby driving the first gear 987 to drive the positioning plate 983 to rotate in 97 through the first driving gear 984, the ring frame 981 drives the brush head assemblies 982 to rotate around the surface of the heat exchanging pipe 323, and further improves the cleaning effect on the heat exchanging pipe 323.
The brush head assembly 982 includes a driving shaft 9821 annularly distributed on the annular frame 981, one end of the driving shaft 9821 facing the inner side of the annular frame 981 is fixed with a brush head 9822, the other end is fixed with a third gear 9823, and the collar 97 is provided with a third transmission gear 9824 matched with the third gear 9823, so that the third gear 9823 drives the driving shaft 9821 to rotate through the third transmission gear 9824 along with the rotation of the annular frame 981 in the collar 97, the brush head 9822 is driven to rotate around the driving shaft 9821 for cleaning, and the surface of the heat exchanging through pipe 323 is cleaned through a plurality of rotation directions, so that the cleaning thoroughness is improved, and the cleaning effect is ensured.
The electrolytic bath is characterized in that an anode plate 101 and a cathode plate 102 for electrolytic reaction are arranged in the electrolytic bath body 1, the anode plate 101 and the cathode plate 102 are vertically and alternately arranged, a circulating liquid uniform distributor 103 connected with a circulating discharge pipe 5 is arranged at the inner top of the electrolytic bath body 1, a plurality of circulating liquid discharge ports 104 are arranged at the bottom of the circulating liquid uniform distributor 103, tar and the like can be generated in the process of flushing the surface of the electrode plate by arranging the circulating liquid uniform distributor 103, the electrolytic process is influenced, meanwhile, a product which is not completely fluorinated is fully contacted with fluorine atoms generated by the electrolysis, so that the fluorination is more thorough, and the reaction efficiency is improved.
The product discharge pipes 7 are connected to respective intermediate tanks 10, which intermediate tanks 10 are pumped to the feed end of the distillation apparatus.
The top of the electrolytic bath body 1 is connected with a tail gas discharge pipe 11.
The left side of the electrolytic bath body 1 is connected with a nitrogen gas replacement pipe 12, and the nitrogen gas replacement pipe 12 is connected to an external nitrogen gas source.
A production method of perfluorinated tributyl amine comprises the following specific steps of S1, replacing air in an electrolytic tank body 1 by nitrogen before reaction, replacing the air with nitrogen, mixing the nitrogen and the nitrogen preliminarily to prepare electrolyte in the electrolytic tank body 1, S2, respectively preparing the tributyl amine and hydrogen fluoride according to the mass ratio of 24-30 kg to 200-230 kg, adding the hydrogen fluoride into the electrolytic tank body 1, adding the tributyl amine, S3, introducing low-voltage current to perform electrolytic replacement reaction, controlling the reaction pressure of the electrolytic tank to be 0.1-1.5 MP and the temperature to be 5-15 ℃, S5, after the electrolysis is completed, performing electrolytic fluorination on the tributyl amine to convert the tributyl amine into perfluorinated tributyl amine, and discharging the perfluorinated tributyl amine from the bottom of the electrolytic tank body 1 to obtain the perfluorinated tributyl amine.
The electrolytic tank body 1 in this embodiment adopts the electrolytic tank body 1 in the prior art, and the electrolysis means are all in the prior art, so the details are not repeated here, the structure of the electrolytic tank body 1 is not expanded in the figure, and the electrolytic fluorination method is adopted, so the reaction is mild and controllable, the process is simple, the efficiency is high, the impurities are few, and the separation is easy.
By adopting the method and the device, the fluorination degree in the reaction process can be improved, and the crude product of the perfluoro tributylamine with the purity of more than 80 percent can be obtained under the conditions of simple reaction raw materials and simple and convenient reaction device.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, and various modifications and variations may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
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