CN115896830A - Reaction kettle and electrochemical reaction device with same - Google Patents
Reaction kettle and electrochemical reaction device with same Download PDFInfo
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- CN115896830A CN115896830A CN202310124012.4A CN202310124012A CN115896830A CN 115896830 A CN115896830 A CN 115896830A CN 202310124012 A CN202310124012 A CN 202310124012A CN 115896830 A CN115896830 A CN 115896830A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 110
- 238000003487 electrochemical reaction Methods 0.000 title claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 66
- 238000003756 stirring Methods 0.000 claims description 12
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 43
- 238000005868 electrolysis reaction Methods 0.000 description 23
- 238000007254 oxidation reaction Methods 0.000 description 15
- 230000003647 oxidation Effects 0.000 description 13
- 238000000034 method Methods 0.000 description 7
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical group CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 238000004128 high performance liquid chromatography Methods 0.000 description 5
- 239000011229 interlayer Substances 0.000 description 5
- SJWFXCIHNDVPSH-UHFFFAOYSA-N octan-2-ol Chemical compound CCCCCCC(C)O SJWFXCIHNDVPSH-UHFFFAOYSA-N 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 238000005070 sampling Methods 0.000 description 5
- 239000007858 starting material Substances 0.000 description 5
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- GDWRKZLROIFUML-UHFFFAOYSA-N 4-phenylbutan-2-ol Chemical compound CC(O)CCC1=CC=CC=C1 GDWRKZLROIFUML-UHFFFAOYSA-N 0.000 description 4
- 125000005233 alkylalcohol group Chemical group 0.000 description 4
- 150000001728 carbonyl compounds Chemical class 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
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Abstract
The invention provides a reaction kettle and an electrochemical reaction device with the same. Wherein, reation kettle includes: the reaction kettle body is provided with an accommodating cavity, and the accommodating cavity is provided with an opening; the kettle cover is covered at the opening and is provided with a first through hole, a second through hole, a liquid inlet hole and a liquid outlet hole; the first electrode penetrates through the first through hole and stretches into the accommodating cavity, and the second electrode penetrates through the second through hole and stretches into the accommodating cavity. By applying the technical scheme of the invention, the problem of long reaction period of the batch reactor in the related technology can be effectively solved.
Description
Technical Field
The invention relates to the field of electrochemical reaction, in particular to a reaction kettle and an electrochemical reaction device with the same.
Background
Among many chemical reactions, the selective oxidation of alkyl alcohols to carbonyl compounds has attracted much attention because of its important application in the fields of pharmaceutical intermediates, chemical material synthesis, flavor industry, food production, and the like. Compared with the traditional alcohol oxidation method, the electrochemical selective alcohol oxidation is concerned about because a metal reagent is not used and the method is green and environment-friendly, and is mainly divided into direct electrochemical alcohol oxidation and indirect electrochemical alcohol oxidation. Direct electrochemical alcohol oxidation, although continuous synthesis has been achieved, has not been widely practiced due to limited substrate applicability. Indirect electrochemical alcohol oxidation research starts earlier and mainly focuses on two-phase electrolysis, and has higher requirements on the electrolyte, so that the electrolysis efficiency is generally lower, and the large-scale electrolysis application is few.
In the related art, the selective oxidation reaction of alkyl alcohol to carbonyl compound is mainly carried out in a batch reactor, such as a conventional box-type electrochemical reactor, a filter press-type electrochemical reactor, etc. The batch reactor has the advantages of longer auxiliary time of batch operation, large equipment specification required by batch amplification, low heat exchange efficiency, long reaction period, low space-time yield and no contribution to large-scale production.
Disclosure of Invention
The invention mainly aims to provide a reaction kettle and an electrochemical reaction device with the same, so as to solve the problem of long reaction period of a batch reactor in the related technology.
In order to achieve the above object, according to one aspect of the present invention, there is provided a reaction tank comprising: the reaction kettle comprises a reaction kettle body and a reaction kettle body, wherein the reaction kettle body is provided with an accommodating cavity which is provided with an opening; the kettle cover is covered at the opening and is provided with a first through hole, a second through hole, a liquid inlet hole and a liquid outlet hole; the first electrode penetrates through the first through hole and stretches into the accommodating cavity, and the second electrode penetrates through the second through hole and stretches into the accommodating cavity.
Further, the reaction kettle also comprises: the liquid inlet pipe penetrates through the liquid inlet hole and extends into the accommodating cavity, the bottom end of the liquid inlet pipe is adjacent to the bottom wall of the accommodating cavity, and a first gap is formed between the bottom end of the liquid inlet pipe and the bottom wall of the accommodating cavity; the drain pipe passes and stretches into to holding the intracavity at the drain hole, and the bottom of drain pipe and the adjacent setting of lower surface of kettle cover and have the second clearance between the bottom of drain pipe and the lower surface of kettle cover.
Further, the reation kettle body includes first sleeve and is located the second sleeve of first sleeve, holds the chamber and is located the second sleeve, forms the intermediate layer space that supplies the medium to flow between first sleeve and the second sleeve, still is provided with on the first sleeve with intermediate layer space respectively the intercommunication medium import and medium export.
Furthermore, the first through holes are multiple, the first through holes are arranged at intervals in the circumferential direction of the kettle cover, the second through holes are multiple, the second through holes are located on the outer sides of the first through holes in the circumferential direction, and the second through holes and the first through holes are arranged in a one-to-one correspondence mode.
Further, each second through hole and the corresponding first through hole are arranged in a staggered mode in the radial direction of the kettle cover.
Furthermore, the first through hole and the second through hole are arc-shaped holes, the second through hole is located on the outer side of the first through hole in the circumferential direction, the first electrode is of an arc-shaped structure matched with the first through hole, and the second electrode is of an arc-shaped structure matched with the second through hole.
Further, still be provided with the third through-hole on the kettle cover, the third through-hole is located the outside of second through-hole and sets up with the second through-hole interval, is provided with the third electrode in the third through-hole, and third electrode and first electrode are the positive pole.
Further, the reaction kettle also comprises: the stirring structure penetrates through the kettle cover and extends into the accommodating cavity; and/or, the reaction kettle further comprises: the thermometer is arranged on the kettle cover in a penetrating way and extends into the accommodating cavity.
According to another aspect of the present invention, there is provided an electrochemical reaction device including: a liquid storage tank; the reaction kettle is the reaction kettle, and a liquid inlet hole of the reaction kettle is communicated with the liquid storage tank; and the discharge box is arranged at the downstream of the reaction kettle, and a liquid outlet hole of the reaction kettle is communicated with the discharge box.
Furthermore, the reaction kettles are arranged in series.
By applying the technical scheme of the invention, the reaction kettle comprises a reaction kettle body and a kettle cover, wherein the reaction kettle body is internally provided with a containing cavity for containing reaction materials, the kettle cover is provided with a first through hole for installing a first electrode and a second through hole for installing a second electrode, the kettle cover is also provided with a liquid inlet hole and a liquid outlet hole, the reaction materials can enter the reaction kettle through the liquid inlet hole, and the reaction materials after electrolysis can be discharged through the liquid outlet hole. Above-mentioned structure makes reation kettle form an inclosed reaction vessel, can carry out the electrolysis to reaction material through first electrode and second electrode, can realize the feeding and the discharge of material through feed liquor hole and play liquid hole to make first electrode and second electrode in the reation kettle just at the during operation, also can realize the feeding and the ejection of compact, thereby can guarantee electrochemical reaction's continuity, help promoting reaction efficiency.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 shows a schematic structural diagram of an embodiment of a reaction vessel according to the invention;
FIG. 2 shows a top view of the cover of the reaction vessel of FIG. 1;
fig. 3 shows a schematic structural view of an embodiment of an electrochemical reaction apparatus according to the present invention.
Wherein the figures include the following reference numerals:
10. a reaction kettle body; 11. a first sleeve; 111. a media inlet; 112. a media outlet; 12. a second sleeve; 121. an accommodating chamber; 13. an interlayer space; 20. a kettle cover; 21. a first through hole; 22. a second through hole; 23. a liquid inlet hole; 24. a liquid outlet hole; 25. a third through hole; 30. a first electrode; 40. a second electrode; 50. a stirring structure; 60. a thermometer; 70. a liquid storage tank; 80. a reaction kettle; 90. a discharge box; 100. a liquid inlet pipe; 200. a liquid outlet pipe.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless it is specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective portions shown in the drawings are not drawn in an actual proportional relationship for the convenience of description. Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, further discussion thereof is not required in subsequent figures.
A continuous stirred reactor system, or called a full-mixing anaerobic reactor, CSTR for short, is an anaerobic treatment technique for making fermentation raw materials and microorganisms in a completely mixed state. The reactor of the present application serves as a reactor in a continuous stirred reactor system for carrying out a selective oxidation reaction of an alkyl alcohol to a carbonyl compound. Specifically, the method comprises the following steps:
as shown in fig. 1 and 2, the reaction vessel of the present embodiment includes: the reaction kettle comprises a reaction kettle body 10, a kettle cover 20, a first electrode 30 and a second electrode 40. The reaction kettle body 10 is provided with an accommodating cavity 121, and the accommodating cavity 121 is provided with an opening; the kettle cover 20 is covered at the opening, and a first through hole 21, a second through hole 22, a liquid inlet hole 23 and a liquid outlet hole 24 are arranged on the kettle cover 20; the polarities of the first electrode 30 and the second electrode 40 are opposite, the first electrode 30 penetrates through the first through hole 21 and extends into the accommodating cavity 121, and the second electrode 40 penetrates through the second through hole 22 and extends into the accommodating cavity 121.
Use the technical scheme of this embodiment, reation kettle includes reation kettle body 10 and kettle cover 20, cavity 121 holds has in the reation kettle body 10, hold cavity 121 and be used for holding dress reaction material, be provided with the first through-hole 21 of installation first electrode 30 and the second through-hole 22 of installation second electrode 40 on the kettle cover 20, still be provided with feed liquor hole 23 and play liquid hole 24 on the kettle cover 20, reaction material can pass through in the feed liquor hole 23 gets into reation kettle, the reaction material that the electrolysis was accomplished can be discharged through going out the liquid hole. Above-mentioned structure makes reation kettle form an inclosed reaction vessel, can carry out the electrolysis to reaction material through first electrode 30 and second electrode 40, can realize the feeding and the discharge of material through feed liquor hole 23 and play liquid hole 24, thereby make first electrode 30 and second electrode 40 in the reation kettle just at the during operation, also can realize the feeding and the ejection of compact, thereby can guarantee electrochemical reaction's continuity, help promoting reaction efficiency.
In order to form a closed reaction vessel in the reaction kettle, the first electrode 30 and the first through hole 21 need to be in sealing engagement, for example, a sealing ring is provided therebetween, and the second electrode 40 and the second through hole 22 need to be in sealing engagement.
As shown in fig. 1 to fig. 3, in the present embodiment, the reaction kettle further includes a liquid inlet pipe 100 and a liquid outlet pipe 200. The liquid inlet pipe 100 penetrates through the liquid inlet hole 23 and extends into the accommodating cavity 121, the bottom end of the liquid inlet pipe 100 is adjacent to the bottom wall of the accommodating cavity 121, and a first gap is formed between the bottom end of the liquid inlet pipe 100 and the bottom wall of the accommodating cavity 121; effluent pipe 200 passes and stretches into in holding chamber 121 at effluent hole 24, and the bottom of effluent pipe 200 sets up adjacent to the lower surface of kettle cover 20 and has the second clearance between the bottom of effluent pipe 200 and the lower surface of kettle cover 20.
In the above-mentioned structure, the bottom of feed liquor pipe 100 and the diapire that holds the chamber 121 are adjacent to be set up and have first clearance between the bottom of feed liquor pipe 100 and the diapire that holds the chamber 121 for the setting is pressed close to the bottom of feed liquor pipe 100 and the diapire that holds the chamber 121. Simultaneously, the bottom of drain pipe 200 and the adjacent setting of lower surface of kettle cover 20 and have the second clearance between the bottom of drain pipe 200 and the lower surface of kettle cover 20, make the bottom of drain pipe 200 be close to kettle cover 20 and set up, thereby make the material can enter into reation kettle's bottom earlier, the reactant liquid level submergence first electrode 30 and second electrode 40 at the in-process that rises gradually, and carry out the electrolysis through first electrode 30 and second electrode 40, the material rethread that the electrolysis was accomplished overflows near the drain pipe 200 that kettle cover 20 set up, obtain the material that the electrolysis was accomplished. This kind of mode of setting makes to have great difference in height between feed liquor pipe 100 and the drain pipe 200 to can guarantee to discharge from drain pipe 200 again after the material electrolysis is accomplished, thereby guarantee to follow the electrolytic effect of drain pipe 200 exhaust material.
It should be noted that the distance of the first gap is between 0.5mm and 50mm, and the distance of the second gap is between 0.3mm and 50 mm.
As shown in fig. 1 and fig. 2, in this embodiment, the reaction kettle body 10 includes a first sleeve 11 and a second sleeve 12 located in the first sleeve 11, the accommodating cavity 121 is located in the second sleeve 12, an interlayer space 13 for flowing a medium is formed between the first sleeve 11 and the second sleeve 12, and the first sleeve 11 is further provided with a medium inlet 111 and a medium outlet 112 respectively communicated with the interlayer space 13. In the above structure, the medium can flow in the interlayer space 13, thereby adjusting the reaction temperature of the reaction vessel body 10. It should be noted that, in this embodiment, the medium circulating in the interlayer space 13 is a heating medium, and the heating medium can raise the reaction temperature of the reaction kettle, thereby further accelerating the reaction rate.
As shown in fig. 1 and fig. 2, in the present embodiment, the first through holes 21 are multiple, the multiple first through holes 21 are arranged at intervals in the circumferential direction of the kettle cover 20, the multiple second through holes 22 are multiple, the multiple second through holes 22 are located at the circumferential outer side of the multiple first through holes 21, and the multiple second through holes 22 and the multiple first through holes 21 are arranged in a one-to-one correspondence. In the above structure, the first through holes 21 are plural, and the first electrodes 30 are plural in one-to-one correspondence with the first through holes. Accordingly, there are a plurality of second through holes 22, and a plurality of second electrodes 40 are provided in one-to-one correspondence with the second through holes 22. The above arrangement allows the first electrode 30 and the second electrode 40 to be arranged in pairs, thereby ensuring the normal progress of the electrochemical reaction. In addition, the first electrode 30 and the second electrode 40 are provided in plural, so that the use time of the first electrode 30 and the second electrode 40 can be ensured, and the frequency of replacing the first electrode 30 and the second electrode 40 can be reduced.
It should be further noted that the first through holes 21 are arranged at intervals in the circumferential direction of the kettle cover 20, and the plurality of second through holes 22 are located at the circumferential outer sides of the plurality of first through holes 21, so that the arrangement of the first electrodes 30 and the second electrodes 40 on the kettle cover 20 is more optimized and reasonable, and the arrangement is helpful for an operator to orderly replace the first electrodes 30 and the second electrodes 40.
As shown in fig. 1 and fig. 2, in the present embodiment, each second through hole 22 and the corresponding first through hole 21 are arranged in a staggered manner in the radial direction of the kettle cover 20. The arrangement mode is beneficial to increasing the facing area of the first electrode 30 and the second electrode 40, thereby being beneficial to improving the electrolysis efficiency of materials.
In the present embodiment, the cross-section of the first electrode 30 and the second electrode 40 may be circular or polygonal.
In other embodiments, the first through hole 21 and the second through hole 22 may be both arc-shaped holes, the second through hole 22 is located at the circumferential outer side of the first through hole 21, the first electrode 30 is an arc-shaped structure disposed in cooperation with the first through hole 21, and the second electrode 40 is an arc-shaped structure disposed in cooperation with the second through hole 22. The structure can ensure the facing area of the first electrode 30 and the second electrode 40, thereby being beneficial to improving the electrolysis efficiency of materials.
As shown in fig. 1 and fig. 2, in the present embodiment, a third through hole 25 is further disposed on the kettle cover 20, the third through hole 25 is located outside the second through hole 22 and spaced from the second through hole 22, a third electrode is disposed in the third through hole 25, and both the third electrode and the first electrode 30 are anodes. In the structure, because the consumption rate of the anode is greater than that of the cathode in the electrolytic reaction, the third through hole 25 is formed in the kettle cover 20, and the third electrode which is the anode is also arranged in the third through hole 25, so that the replacement frequency of the anode is reduced, and the use experience of the reaction kettle is improved.
As shown in fig. 1, in this embodiment, the reaction kettle further includes a stirring structure 50, and the stirring structure 50 is disposed on the kettle cover 20 and extends into the accommodating cavity 121. In the above-mentioned structure, because the inlet pipe has in the reation kettle, therefore the reaction mass that the electrolysis is good needs the misce bene with the reaction mass that newly gets into in the reation kettle for the material that newly gets into in the reation kettle carries out abundant contact with first electrode 30 and second electrode 40, thereby makes the reaction mass that newly gets into in the reation kettle can be electrolyzed rapidly. The stirring structure 50 can improve the mixing uniformity of the electrolyzed reaction material and the reaction material newly entering the reaction kettle.
It should be noted that, stirring structure 50 includes the agitator motor that sets up on kettle cover 20, the puddler of being connected with agitator motor's axis of rotation drive and sets up the stirring vane on the puddler, and stirring vane includes the multilayer, and multilayer stirring vane sets up at the axial direction interval of puddler to guarantee stirring structure 50's stirring effect.
As shown in fig. 3, in this embodiment, the reaction kettle further includes a thermometer 60, and the thermometer 60 is disposed on the kettle cover 20 and extends into the accommodating cavity 121. In the above structure, the thermometer 60 can monitor the reaction temperature of the liquid in the reaction kettle in real time, and the operator can adjust the temperature of the heating medium according to the temperature indication of the thermometer 60, thereby ensuring that the reaction is carried out at a predetermined temperature.
As shown in fig. 3, the present application also provides an electrochemical reaction device, and an embodiment of the electrochemical reaction device of the present application includes: a liquid storage tank 70, a reaction kettle 80 and a discharge tank 90. Wherein, the reaction kettle 80 is the reaction kettle, and the liquid inlet hole 23 of the reaction kettle 80 is communicated with the liquid storage tank 70; the discharge box 90 is arranged at the downstream of the reaction kettle 80, and the liquid outlet hole 24 of the reaction kettle 80 is communicated with the discharge box 90. In the above structure, the reaction material is temporarily stored in the liquid storage tank 70, and the liquid inlet pipe 100 can communicate the material storage tank 70 and the reaction kettle 80. After the reaction materials enter the reaction kettle 80, electrolysis is carried out through the first electrode 30 and the second electrode 40, and the materials after electrolysis overflow through the liquid outlet pipe 200 arranged close to the kettle cover 20 to obtain the materials after electrolysis. The above-described electrochemical reaction apparatus enables continuous progress of the reaction by continuous feeding and continuous discharging, as compared with the conventional apparatus in which a predetermined volume of reaction materials is reacted for a predetermined period of time and then discharged together.
It should be noted that the material in the liquid storage tank 70 may be fed into the reaction kettle 80 by a material pump. The material in the reaction kettle 80 can also be sent into the discharge box 90 through a material pump.
As shown in fig. 3, in the present embodiment, a plurality of reaction vessels 80 are provided, and a plurality of reaction vessels 80 are provided in series. In the above structure, a plurality of reaction kettles 80 may be arranged in series, and the effluent pipe 200 of the most downstream reaction kettle 80 may be communicated with the discharge box 90. The arrangement mode can increase the material handling capacity of the electrochemical reaction device and can ensure the electrolysis effect on reaction materials.
The examples of selective oxidation of alkyl alcohol to carbonyl compounds using the electrochemical reaction apparatus of the above examples are as follows:
the first embodiment is as follows: continuous electric reaction for oxidation of sec-octanol
1. Preparing materials: under room temperature conditions, solution 1 was prepared: 40g of secondary octanol and 0.05eq TEMPO are dissolved in 533ml THF, and the solution is clear for standby; preparing a solution 2:238g2.4eq tetrabutylammonium bromide dissolved in 1067ml of 1% Na 2 HPO 4 Dissolving in water solution;
2. electrolysis: the continuous electrochemical CSTR device is adopted: the liquid holdup of a single CSTR is 400ml, two CSTRs are connected in series, the cathode and anode are made of graphite, and the current density is 20mA/cm 2 The inter-polar distance is 0.2cm, the temperature is controlled to be 25-35 ℃, each CSTR electrolyzes 2F, the total reaction time is 4F, and the liquid outlet sampling tracking is carried out.
3. Calibrating yield: transferring the reacted system to a receiving kettle for temporary storage, and separately temporarily storing the materials with the middle two reserved volumes to obtain a stable sample calibration yield; HPLC showed about 5.2% starting material remaining, product external standard yield 87.5%; the reactor space-time yield was 6.2 g/L.multidot.h, which is about 3 times that of the batch reactor.
Example two: continuous electric reaction for oxidation of sec-octanol
1. Preparing materials: at room temperature, solution 1:80g of secondary octanol and 0.05eq TEMPO were dissolved in 1066ml of THF and the solution was clear for further use; preparing a solution 2:476g2.4eq tetrabutylammonium bromide dissolved in 2134ml of 1% Na 2 HPO 4 Dissolving in water solution;
2. electrolysis: by usingThe continuous electrochemical CSTR apparatus described above: the liquid holdup of a single CSTR is 400ml, four CSTRs are connected in series, the cathode and anode are made of graphite, and the current density is 20mA/cm 2 The distance between the electrodes is 0.2cm, the temperature is controlled to be 25-35 ℃, each stage of CSTR electrolyzes 1F, the total reaction time is 4F, and the sampling tracking is carried out at the liquid outlet.
3. Calibrating yield: transferring the reacted system to a receiving kettle for temporary storage, and separately temporarily storing the materials with the middle two reserved volumes to obtain a stable sample calibration yield; HPLC showed approximately 0.3% starting material remaining, with an external standard yield of 91.8% for the product.
Example three: continuous electric reaction for oxidation of sec-octanol
1. Preparing materials: under room temperature conditions, solution 1 was prepared: 40g of secondary octanol and 0.05eq TEMPO were dissolved in 533ml of THF, and the solution was clear for further use; preparing a solution 2:238g2.4eq tetrabutylammonium bromide dissolved in 1067ml of 1% Na 2 HPO 4 Dissolving in water solution;
2. electrolysis: the continuous electrochemical CSTR device is adopted: the liquid holdup of a single CSTR is 400ml, two CSTRs are connected in series, the cathode and anode are made of three-dimensional carbon felt electrodes, the electrode is a circular ring-shaped electrode, the inner ring is a cathode, the outer ring is an anode as shown in the example of figure 2, the distance between the electrodes is 1.0cm, the outer ring is tightly attached to the wall of the kettle, and the current density is 20mA/cm 2 The distance between poles is 0.2cm, the temperature is controlled to be 25-35 ℃, each CSTR electrolyzes 2F, the total reaction time is 4F, and the sampling tracking is carried out at the liquid outlet.
3. Calibrating yield: transferring the reacted system to a receiving kettle for temporary storage, and separately temporarily storing the materials with the middle two reserved volumes to obtain a stable sample calibration yield; HPLC showed starting material remaining about 4.9%, external standard yield of product 81.1%.
Example four: continuous electric reaction for oxidation of sec-octanol
1. Preparing materials: under room temperature conditions, solution 1 was prepared: 40g of sec-octanol and 0.05 gDissolving eqTEMPO in 533ml of THF, and dissolving for later use; preparing a solution 2:238g2.4eq tetrabutylammonium bromide dissolved in 1067ml of 1% Na 2 HPO 4 Dissolving in water solution;
2. electrolysis: the continuous electrochemical CSTR device is adopted: the liquid holdup of a single CSTR is 400ml, three CSTRs are connected in series, the cathode and anode are made of graphite rod electrodes, the current density of the first stage CSTR is 20mA/cm < 2 >, and the current density of the second stage CSTR is 10mA/cm 2 Third stage CSTR Current Density 10mA/cm 2 The distance between the electrodes is 0.2cm, the temperature is controlled to be 25-35 ℃, the first stage CSTR electrolyzes 2F, the second stage CSTR electrolyzes 1F, the total reaction time is 4F, and the sampling tracking is carried out at the liquid outlet.
3. Calibration yield: transferring the reacted system to a receiving kettle for temporary storage, and separately temporarily storing the materials with the middle two reserved volumes to obtain a stable sample calibration yield; HPLC showed about 2.5% starting material remaining, with an external standard yield of 87.5% for the product.
Example five: 4-phenyl-2-butanol oxidation continuous electric reaction
1. Preparing materials: under room temperature conditions, solution 1: dissolving 46.2g of 4-phenyl-2 butanol and 0.05eq TEMPO in 533ml THF, and dissolving clear for standby; preparing a solution 2:238g2.4eq tetrabutylammonium bromide dissolved in 1067ml of 1% Na 2 HPO 4 Dissolving in water solution;
2. electrolysis: the continuous electrochemical CSTR device is adopted: the liquid holdup of a single CSTR is 400ml, two CSTRs are connected in series, the cathode and anode are made of graphite, and the current density is 20mA/cm 2 The distance between poles is 0.2cm, the temperature is controlled to be 25-35 ℃, each CSTR electrolyzes 2F, the total reaction time is 4F, and the sampling tracking is carried out at the liquid outlet.
3. Calibration yield: transferring the reacted system to a receiving kettle for temporary storage, and separately temporarily storing the materials with the middle two reserved volumes to obtain a stable sample calibration yield; HPLC showed starting material to be about 2.1% remaining, with an external standard yield of 81.4% for the product.
In the description of the present invention, it is to be understood that the orientation or positional relationship indicated by the orientation words such as "front, rear, upper, lower, left, right", "lateral, vertical, horizontal" and "top, bottom", etc. are usually based on the orientation or positional relationship shown in the drawings, and are only for convenience of description and simplicity of description, and in the case of not making a reverse description, these orientation words do not indicate and imply that the device or element being referred to must have a specific orientation or be constructed and operated in a specific orientation, and therefore, should not be considered as limiting the scope of the present invention; the terms "inner and outer" refer to the inner and outer relative to the profile of the respective component itself.
For ease of description, spatially relative terms such as "over 8230 \ 8230;,"' over 8230;, \8230; upper surface "," above ", etc. may be used herein to describe the spatial relationship of one device or feature to another device or feature as shown in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if a device in the figures is turned over, devices described as "above" or "on" other devices or configurations would then be oriented "below" or "under" the other devices or configurations. Thus, the exemplary terms "at 8230; \8230; 'above" may include both orientations "at 8230; \8230;' above 8230; 'at 8230;' below 8230;" above ". The device may be otherwise variously oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
It should be noted that the terms "first", "second", and the like are used to define the components, and are only used for convenience of distinguishing the corresponding components, and unless otherwise stated, the terms have no special meaning, and therefore, the scope of the present invention should not be construed as being limited.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A reaction kettle, comprising:
the reaction kettle comprises a reaction kettle body (10) and a reaction kettle body, wherein the reaction kettle body is provided with a containing cavity (121), and the containing cavity (121) is provided with an opening;
the kettle cover (20) is covered at the opening, and a first through hole (21), a second through hole (22), a liquid inlet hole (23) and a liquid outlet hole (24) are formed in the kettle cover (20);
the electrode structure comprises a first electrode (30) and a second electrode (40), wherein the polarities of the first electrode (30) and the second electrode (40) are opposite, the first electrode (30) penetrates through the first through hole (21) and stretches into the accommodating cavity (121), and the second electrode (40) penetrates through the second through hole (22) and stretches into the accommodating cavity (121).
2. The reactor of claim 1, further comprising:
the liquid inlet pipe (100) penetrates through the liquid inlet hole (23) and extends into the accommodating cavity (121), the bottom end of the liquid inlet pipe (100) is arranged adjacent to the bottom wall of the accommodating cavity (121), and a first gap is formed between the bottom end of the liquid inlet pipe (100) and the bottom wall of the accommodating cavity (121);
and the liquid outlet pipe (200) penetrates through the liquid outlet hole (24) and extends into the accommodating cavity (121), the bottom end of the liquid outlet pipe (200) is adjacent to the lower surface of the kettle cover (20), and a second gap is formed between the bottom end of the liquid outlet pipe (200) and the lower surface of the kettle cover (20).
3. The reaction kettle according to claim 1, wherein the reaction kettle body (10) comprises a first sleeve (11) and a second sleeve (12) located in the first sleeve (11), the accommodating cavity (121) is located in the second sleeve (12), a sandwich space (13) for medium flowing is formed between the first sleeve (11) and the second sleeve (12), and the first sleeve (11) is further provided with a medium inlet (111) and a medium outlet (112) respectively communicated with the sandwich space (13).
4. The reaction kettle according to claim 1, wherein the first through holes (21) are plural, the plural first through holes (21) are arranged at intervals in the circumferential direction of the kettle cover (20), the plural second through holes (22) are plural, the plural second through holes (22) are located at the circumferential outer side of the plural first through holes (21), and the plural second through holes (22) are arranged in one-to-one correspondence with the plural first through holes (21).
5. The reactor according to claim 4, wherein each of the second through holes (22) is offset from the corresponding first through hole (21) in a radial direction of the vessel cover (20).
6. The reaction kettle according to claim 4, wherein the first through hole (21) and the second through hole (22) are both arc-shaped holes, the second through hole (22) is located at the circumferential outer side of the first through hole (21), the first electrode (30) is a first arc-shaped structure matched with the first through hole (21), and the second electrode (40) is a second arc-shaped structure matched with the second through hole (22).
7. The reaction kettle according to claim 4, wherein a third through hole (25) is further formed in the kettle cover (20), the third through hole (25) is located on the outer side of the second through hole (22) and spaced from the second through hole (22), a third electrode is arranged in the third through hole (25), and the third electrode and the first electrode (30) are both anodes.
8. The reactor of claim 1, further comprising:
the stirring structure (50) penetrates through the kettle cover (20) and extends into the accommodating cavity (121);
and/or the presence of a gas in the atmosphere,
the thermometer (60) penetrates through the kettle cover (20) and extends into the accommodating cavity (121).
9. An electrochemical reaction device, comprising:
a reservoir (70);
a reaction kettle (80) as claimed in any one of claims 1 to 8, wherein a liquid inlet hole (23) of the reaction kettle (80) is communicated with the liquid storage tank (70);
and the discharge box (90) is arranged at the downstream of the reaction kettle (80), and the liquid outlet hole (24) of the reaction kettle (80) is communicated with the discharge box (90).
10. The electrochemical reaction apparatus according to claim 9, wherein the reaction vessel (80) is provided in plurality, and the plurality of reaction vessels (80) are arranged in series.
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| CN202310124012.4A CN115896830A (en) | 2023-02-16 | 2023-02-16 | Reaction kettle and electrochemical reaction device with same |
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| CN202310124012.4A CN115896830A (en) | 2023-02-16 | 2023-02-16 | Reaction kettle and electrochemical reaction device with same |
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