CN109055968B - Organic electro-synthesis electrolysis device - Google Patents

Organic electro-synthesis electrolysis device Download PDF

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Publication number
CN109055968B
CN109055968B CN201810761754.7A CN201810761754A CN109055968B CN 109055968 B CN109055968 B CN 109055968B CN 201810761754 A CN201810761754 A CN 201810761754A CN 109055968 B CN109055968 B CN 109055968B
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electrolyzer
cover
electrolytic cell
cover body
organic electrosynthesis
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CN109055968A (en
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樊陈莉
张强
高天铱
魏程
黄升升
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Wuhu Institute of Technology
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Wuhu Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B3/00Electrolytic production of organic compounds
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B9/00Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • C25B9/17Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof

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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)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)

Abstract

The invention discloses an organic electrosynthesis electrolysis device, wherein an electrolytic tank is coaxially fixed on a magnetic stirrer body, a cover body covers the opening position of the electrolytic tank, interlayers which are mutually communicated are arranged inside the side wall and the bottom wall of the electrolytic tank, and heat conducting liquid is filled in the interlayers; wherein, the center position of the bottom of the cover body is fixedly connected with a fixed plate, the electrode mechanism is fixedly connected on the fixed plate, a wire harness for electrically connecting the electrode mechanism penetrates through the cover body, the top of the interlayer is provided with a liquid inlet and an air outlet, and the inner bottom of the electrolytic bath is provided with a magneton matched with the magnetic stirrer body; the outside of electrolysis trough is provided with constant temperature heating device, is provided with electrothermal tube and thermal resistance on the constant temperature heating device, and electrothermal tube and thermal resistance all stretch into in the heat-conducting liquid and sealed rigid coupling on the electrolysis trough from the outer wall of electrolysis trough, and the thermometer runs through the lid and goes deep into to the electrolysis trough in. The organic electrosynthesis electrolysis device can provide a constant-temperature electrolysis environment and stir the electrolyte.

Description

Organic electro-synthesis electrolysis device
Technical Field
The invention relates to laboratory instruments and equipment, in particular to an organic electrosynthesis electrolyzer.
Background
The organic electrochemical synthesis technology is widely applied to various fields of national economy, and compared with the conventional chemical synthesis method, the method has the advantages of high product purity, less environmental pollution, short process flow, capability of operating at normal pressure and normal temperature and the like, and is a high-efficiency and high-selectivity synthesis method.
Laboratory studies of organic electrochemical synthesis techniques typically use small electrolytic cells as the vessels for organic electrochemical reactions. The commonly used cells have some drawbacks, such as the cells being open, not completely sealed, the reaction solution being exposed to air; the electrolytic cell has no corresponding gas circuit, and the solution can not be aerated in the experimental process; the design of the electrolytic cell is unreasonable, and the structure of the cell body is complex; the electrode spacing is fixed and is not easy to adjust; the solution in the electrolytic bath can not react under the condition of constant temperature, the reaction process can not be stirred, and the electrolytic efficiency is low.
Disclosure of Invention
The invention aims to provide an organic electrosynthesis electrolyzer, which is carried out in a closed environment and can provide a constant-temperature electrolysis environment to stir an electrolyte.
In order to achieve the above object, the present invention provides an organic electrosynthesis electrolyzer comprising: the electrolytic cell is coaxially fixed on the magnetic stirrer body, the cover body covers the opening of the electrolytic cell, interlayers which are mutually communicated are arranged inside the side wall and the bottom wall of the electrolytic cell, and heat conducting liquid is filled in the interlayers; the center of the bottom of the cover body is fixedly connected with a fixed plate, the electrode mechanism is fixedly connected to the fixed plate, a wire harness for electrically connecting the electrode mechanism penetrates through the cover body, the top of the interlayer is provided with a liquid inlet and an air outlet, and the inner bottom of the electrolytic bath is provided with a magneton matched with the magnetic stirrer body; the electrolytic cell is characterized in that a constant-temperature heating device is arranged outside the electrolytic cell, an electric heating tube and a thermal resistor are arranged on the constant-temperature heating device, the electric heating tube and the thermal resistor both extend into the heat-conducting liquid from the outer wall of the electrolytic cell and are fixedly connected to the electrolytic cell in a sealed mode, and the thermometer penetrates through the cover body and extends into the electrolytic cell.
Preferably, be provided with intake pipe, conduit, outlet duct and the sleeve pipe that link up from top to bottom all on the lid, the thermometer inserts the sleeve pipe is deepened in the electrolysis trough, the pencil runs through the conduit setting, the outer end detachably cover of outlet duct is equipped with the latex headgear, the outer end of intake pipe communicates in taking out the gas inflation mechanism.
Preferably, the outer ends of the sleeve and the conduit are respectively sleeved with a part of latex tube.
Preferably, the two electrode plates are located on two sides of the fixing plate, and a fixing screw penetrates through the fixing plate and the two electrode plates to fix the two electrode plates on the fixing plate.
Preferably, the material of set screw is high temperature resistant silica gel.
Preferably, a plurality of position adjusting plates are arranged between the electrode plate and the fixing plate, mounting holes matched with the fixing screws are formed in the position adjusting plates, and the thickness of each position adjusting plate is 1-5 mm.
Preferably, the cover body is in a circular truncated cone shape, the diameter of the horizontal section of the cover body is gradually reduced from top to bottom, and the opening position of the electrolytic cell is meshed with the cover body.
Preferably, the position where the cover body is meshed with the electrolytic bath is set to be a frosted surface.
Preferably, the outer sleeve of the electrolytic cell is provided with a silica gel sleeve with a bottom, the thickness of the silica gel sleeve is not less than 2 mm.
Preferably, the lid is made of PP, and a handle is arranged on the lid.
Preferably, the heat conducting liquid is water or silicone oil.
According to the technical scheme, the electrolytic cell is coaxially fixed on the magnetic stirrer body, the cover body covers the opening of the electrolytic cell, interlayers which are communicated with each other are arranged inside the side wall and the bottom wall of the electrolytic cell, and heat-conducting liquid is filled in the interlayers; the center of the bottom of the cover body is fixedly connected with a fixed plate, the electrode mechanism is fixedly connected to the fixed plate, a wire harness for electrically connecting the electrode mechanism penetrates through the cover body, the top of the interlayer is provided with a liquid inlet and an air outlet, and the inner bottom of the electrolytic bath is provided with a magneton matched with the magnetic stirrer body; the electrolytic cell is characterized in that a constant-temperature heating device is arranged outside the electrolytic cell, an electric heating tube and a thermal resistor are arranged on the constant-temperature heating device, the electric heating tube and the thermal resistor both extend into the heat-conducting liquid from the outer wall of the electrolytic cell and are fixedly connected to the electrolytic cell in a sealed mode, and the thermometer penetrates through the cover body and extends into the electrolytic cell. During the use, at first to leading-in electrolyte in the electrolysis trough, and in thermometer temperature measurement end and electrode mechanism can immerse electrolyte, provide the electrothermal tube heating through constant temperature heating device, transmit the temperature to electrolyte in making the temperature in the electrolyte reach the definite value after the electrothermal tube heating, and read through the thermometer, until electrolyte at the temperature range of needs can, it is movable in electrolyte to drive the magnon through magnetic stirrers body, thereby reach the purpose of stirring, whole electrolysis process is gone on in inclosed environment through the lid, can avoid the influence of air to electrolytic solution.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic view showing the overall structure of a preferred embodiment of an organic electrosynthesis electrolyzer of the present invention;
FIG. 2 is a schematic view showing the overall structure of a preferred embodiment of the cover and the electrode mechanism portion in the present invention;
FIG. 3 is a schematic cross-sectional view of a preferred embodiment of a portion of an electrode mechanism of the present invention;
fig. 4 is a schematic cross-sectional view of a preferred embodiment of the position-adjusting plate of the present invention.
Description of the reference numerals
1 electrolytic cell 2 cover
3 electrode plate 4 heat-conducting liquid
5 electric heating tube 6 silica gel cover
7 exhaust port 8 thermal resistor
9 magneton 10 liquid inlet
11 thermometer 12 magnetic stirrer body
13 air inlet pipe and 14 conduit
15 latex tube 16 handle
17 latex headgear 18 outlet duct
19 fixing plate 20 mounting hole
21 position adjusting plate 22 harness
23 casing 24 fixing screw
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
In the present invention, unless otherwise specified, directional words included in terms such as "upper, lower, left, right, front, rear, inner, and outer" and the like merely represent the directions of the terms in a normal use state or are colloquially known by those skilled in the art, and should not be construed as limiting the terms.
Referring to fig. 1 to 4, an organic electrosynthesis electrolyzer comprising: the electrolytic cell comprises an electrolytic cell 1, a cover body 2, an electrode mechanism, a thermometer 11 and a magnetic stirrer body 12, wherein the electrolytic cell 1 is coaxially fixed on the magnetic stirrer body 12, the cover body 2 covers the opening position of the electrolytic cell 1, interlayers which are mutually communicated are arranged inside the side wall and the bottom wall of the electrolytic cell 1, and heat-conducting liquid 4 is filled in the interlayers; a fixing plate 19 is fixedly connected to the center of the bottom of the cover body 2, the electrode mechanism is fixedly connected to the fixing plate 19, a wire harness 22 for electrically connecting the electrode mechanism penetrates through the cover body 2, a liquid inlet 10 and an air outlet 7 are arranged at the top of the interlayer, and a magneton 9 matched with the magnetic stirrer body 12 is arranged at the inner bottom of the electrolytic cell 1; the electrolytic cell comprises an electrolytic cell 1 and is characterized in that a constant-temperature heating device is arranged outside the electrolytic cell 1, an electric heating tube 5 and a thermal resistor 8 are arranged on the constant-temperature heating device, the electric heating tube 5 and the thermal resistor 8 both extend into the heat-conducting liquid 4 from the outer wall of the electrolytic cell 1 and are fixedly connected to the electrolytic cell 1 in a sealing mode, and a thermometer 11 penetrates through a cover body 2 and extends into the electrolytic cell 1.
Through the implementation of the technical scheme, the electrolytic tank 1 is coaxially fixed on the magnetic stirrer body 12, the cover body 2 covers the opening position of the electrolytic tank 1, interlayers which are mutually communicated are arranged inside the side wall and the bottom wall of the electrolytic tank 1, and heat-conducting liquid 4 is filled in the interlayers; a fixing plate 19 is fixedly connected to the center of the bottom of the cover body 2, the electrode mechanism is fixedly connected to the fixing plate 19, a wire harness 22 for electrically connecting the electrode mechanism penetrates through the cover body 2, a liquid inlet 10 and an air outlet 7 are arranged at the top of the interlayer, and a magneton 9 matched with the magnetic stirrer body 12 is arranged at the inner bottom of the electrolytic cell 1; the electrolytic cell comprises an electrolytic cell 1 and is characterized in that a constant-temperature heating device is arranged outside the electrolytic cell 1, an electric heating tube 5 and a thermal resistor 8 are arranged on the constant-temperature heating device, the electric heating tube 5 and the thermal resistor 8 both extend into the heat-conducting liquid 4 from the outer wall of the electrolytic cell 1 and are fixedly connected to the electrolytic cell 1 in a sealing mode, and a thermometer 11 penetrates through a cover body 2 and extends into the electrolytic cell 1. During the use, at first to leading-in electrolyte in the electrolysis trough 1, and 11 temperature measurement ends of thermometer and electrode mechanism can dip in electrolyte, provide electrothermal tube 5 heating through constant temperature heating device, electrothermal tube 5 heats the back and transmits the temperature to electrolyte in making the temperature in the electrolyte reach the definite value, and read through thermometer 11, until electrolyte in the temperature range of needs can, drive magnetism son 9 through magnetic stirrers body 12 and move about in electrolyte, thereby reach the purpose of stirring, whole electrolysis process is gone on in inclosed environment through lid 2 lid, can avoid the influence of air to electrolytic solution.
In this embodiment, in order to have more electrolysis environments and facilitate the fixing of the wiring harness 22 and the thermometer 11, it is preferable that the cover body 2 is provided with an air inlet pipe 13, a conduit 14, an air outlet pipe 18 and a sleeve 23 which are all vertically penetrated, the thermometer 11 is inserted into the sleeve 23 and goes deep into the electrolytic bath 1, the wiring harness 22 is arranged by penetrating the conduit 14, the outer end of the air outlet pipe 18 is detachably sleeved with a latex head cover 17, and the outer end of the air inlet pipe 13 is communicated with the pump and inflator mechanism. The gas outlet pipe 18 is a gas outlet pipe during gas phase reaction, if the system requires no water, a drying pipe can be connected to the gas outlet pipe 18, and waste gas is discharged through the drying pipe; if the high-temperature electrolyte is gasified, the gas outlet pipe 18 can be connected with a condensing pipe, and the gasified electrolyte is condensed back to the electrolytic tank 1; if the system is required to be closed or anhydrous and oxygen-free, the air outlet pipe 18 is connected with the latex head cover 17, and the latex head cover 17 can indicate the pressure change condition of the system when the system is vacuumized and filled with nitrogen. Taking the electrolysis reaction of the anhydrous anaerobic system as an example, the air inlet pipe 13 is connected with a nitrogen/vacuum pipe, a vacuum pump is started, vacuum pumping is carried out, the latex head is shrunken, nitrogen is filled, and the latex head is recovered. Vacuumizing and filling nitrogen for more than three times, and the system is basically anhydrous and anaerobic. Vacuumizing and filling nitrogen are performed in a vacuumizing and inflating mechanism, and the vacuumizing and inflating mechanism at least comprises a vacuum pump and a nitrogen inflating pump.
In this embodiment, in order to further increase the stability of the fixing of the thermometer 11 and the lead, it is preferable that the sleeve 23 and the outer end of the lead 14 are each sleeved with a portion of the latex tube 15. The diameter of the latex tube 15 is smaller than the diameter of the corresponding thermometer 11 and the wire, and the thermometer 11 and the wire harness 22 are elastically bound by the elastic force of the latex tube 15 so as to play a role of fixing.
In this embodiment, in order to further provide a detachable fixing manner of the electrode pads 3, preferably, two electrode pads 3 are located at two sides of the fixing plate 19, and fixing screws 24 penetrate through the fixing plate 19 and the two electrode pads 3 to fix the two electrode pads 3 on the fixing plate 19.
In this embodiment, in order to prevent the fixing screw 24 from deforming at high temperature and affecting the fixing effect, the material of the fixing screw 24 is preferably high temperature resistant silica gel.
In this embodiment, in order to adjust the distance between the electrode plates 3 in an equal amount, it is preferable that a plurality of position adjustment plates 21 are disposed between the electrode plates 3 and the fixing plate 19, the position adjustment plates 21 are provided with mounting holes 20 matched with the fixing screws 24, and the thickness of the position adjustment plates 21 is 1-5 mm. The distance between the electrode plates 3 is determined according to the number of the position adjusting plates 21, and the positioning device is convenient, rapid and accurate.
In this embodiment, in order to further increase the stability of the cover 2 covering the opening of the electrolytic cell 1, it is preferable that the cover 2 is of a truncated cone shape, the horizontal cross-sectional diameter is gradually reduced from the top to the bottom, and the opening of the electrolytic cell 1 is engaged with the cover 2.
In this embodiment, in order to further increase the stability and sealing property of the cover 2 at the opening position of the electrolytic cell 1, it is preferable that the position where the cover 2 engages with the electrolytic cell 1 is a frosted surface.
In this embodiment, in order to further provide a good heat preservation effect for the heat conducting liquid 4, it is preferable that the outer sleeve of the electrolytic bath 1 is provided with a bottomed silica gel sleeve 6 having a thickness of not less than 2 mm.
In this embodiment, in order to facilitate the operation of the lid 2, it is preferable that the material of the lid 2 is PP, and the handle 16 is provided on the lid 2.
In this embodiment, in order to provide more choices of the heat conductive liquid 4 according to different temperature requirements, it is preferable that the heat conductive liquid 4 is water or silicone oil. The added silicone oil can give higher temperature and is suitable for some high-temperature electrolytic reactions.
The preferred embodiments of the present invention have been described in detail with reference to the accompanying drawings, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.

Claims (9)

1. An organic electrosynthesis electrolyzer, said organic electrosynthesis electrolyzer comprising: the electrolytic cell comprises an electrolytic cell (1), a cover body (2), an electrode mechanism, a thermometer (11) and a magnetic stirrer body (12), wherein the electrolytic cell (1) is coaxially fixed on the magnetic stirrer body (12), the cover body (2) covers the opening of the electrolytic cell (1), interlayers which are mutually communicated are arranged inside the side wall and the bottom wall of the electrolytic cell (1), and heat-conducting liquid (4) is filled in the interlayers; wherein,
a fixed plate (19) is fixedly connected to the center of the bottom of the cover body (2), the electrode mechanism is fixedly connected to the fixed plate (19), a wire harness (22) for electrically connecting the electrode mechanism penetrates through the cover body (2) to be arranged, a liquid inlet (10) and an air outlet (7) are arranged at the top of the interlayer, and a magneton (9) matched with the magnetic stirrer body (12) is arranged at the inner bottom of the electrolytic tank (1);
a constant-temperature heating device is arranged outside the electrolytic tank (1), an electric heating tube (5) and a thermal resistor (8) are arranged on the constant-temperature heating device, the electric heating tube (5) and the thermal resistor (8) extend into the heat-conducting liquid (4) from the outer wall of the electrolytic tank (1) and are fixedly connected to the electrolytic tank (1) in a sealing manner, and the thermometer (11) penetrates through the cover body (2) and extends into the electrolytic tank (1);
the two electrode plates (3) are positioned on two sides of the fixing plate (19), and fixing screws (24) penetrate through the fixing plate (19) and the two electrode plates (3) to fix the two electrode plates (3) on the fixing plate (19);
a plurality of position adjusting plates (21) are arranged between the electrode plate (3) and the fixing plate (19), mounting holes (20) matched with the fixing screws (24) are formed in the position adjusting plates (21), and the thickness of the position adjusting plates (21) is 1-5 mm.
2. The organic electrosynthesis electrolyzer of claim 1, wherein said cover (2) is provided with an air inlet tube (13), a conduit (14), an air outlet tube (18) and a sleeve (23) all extending vertically therethrough, said thermometer (11) is inserted into said sleeve (23) and extends into said electrolyzer (1), said wiring harness (22) is disposed through said conduit (14), the outer end of said air outlet tube (18) is detachably sleeved with a latex headgear (17), and the outer end of said air inlet tube (13) is communicated with an air pumping and inflating mechanism.
3. The organic electrosynthesis electrolyzer of claim 2, characterized in that the external ends of said bushing (23) and conduit (14) are each sheathed with a portion of latex tube (15).
4. The organic electrosynthesis electrolyzer of claim 1, wherein said set screws (24) are made of high temperature resistant silica gel.
5. The organic electrosynthesis electrolyzer of claim 1, characterized in that said cover (2) is of the truncated cone type with a horizontal section diameter that decreases progressively from top to bottom, the open position of said electrolyzer (1) engaging said cover (2).
6. An organic electrosynthesis electrolysis device as defined in claim 5 wherein the location where said cover (2) engages said cell (1) is provided as a frosted surface.
7. The organic electrosynthesis electrolyzer of claim 1, characterized in that the external jacket of said electrolyzer (1) is equipped with a bottomed silicone jacket (6) having a thickness not less than 2 mm.
8. The organic electrosynthesis electrolyzer of claim 1, wherein said cover (2) is made of PP and said cover (2) is provided with a handle (16).
9. The organic electrosynthesis electrolyzer of claim 1, characterized in that said thermally conductive liquid (4) is water or silicone oil.
CN201810761754.7A 2018-07-12 2018-07-12 Organic electro-synthesis electrolysis device Active CN109055968B (en)

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