CN216473513U - Device for synthesizing amide organic micromolecules through electrocatalysis - Google Patents
Device for synthesizing amide organic micromolecules through electrocatalysis Download PDFInfo
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Abstract
The utility model discloses a device for synthesizing amide organic micromolecules by electrocatalysis, the outlet of a raw material tank is connected with the inlet of a reaction device through a pipeline, a pH sensor, a temperature sensor and a pressure sensor are respectively connected with the reaction device, an anode component, a cathode component and a reference electrode component are arranged in the reaction device, a membrane component is arranged between the anode component and the cathode component, the anode component, the cathode component and the reference electrode component form a three-electrode system and are connected with external electric control equipment arranged outside the reaction device, a stirring part is arranged in the reaction device, the first outlet of the reaction device is connected with a gas product storage tank through a pipeline so as to collect gas products, such as hydrogen and oxygen which are produced along with the reaction; and a second outlet of the reaction device is connected with the separation rectifying tower through a pipeline, and the separation rectifying tower is connected with the first collecting tower and the second collecting tower through pipelines. The utility model discloses use three electrode system to carry out the constant potential reaction to the raw materials to the amide compound is synthesized to the electrochemistry technology, has realized the maximize that the raw materials utilized, has greatly reduced material cost.
Description
Technical Field
The utility model relates to an electrocatalysis amide organic small molecule synthesizer, more specifically say, relate to one kind and use formic acid and nitrogen oxide as the raw materials through the synthetic organic small molecule of coreduction reaction (formamide), provide the electrocatalysis device of one kind.
Background
Formamide is an important basic chemical raw material and is widely applied to the fields of medicine industry, biology and the like. Currently, there are two main industrial methods for the synthesis of formamide. Firstly, mixing carbon monoxide and ammonia gas, taking sodium methoxide as a catalyst, and directly synthesizing formamide by a one-pot method under the conditions of high temperature and high pressure (0.8-1.7 MPa, 348-353K); secondly, carbon monoxide and methanol are used as raw materials, methyl formate is firstly obtained at high temperature and high pressure (10-30 MPa, 353-373K) in the presence of sodium methoxide, and the methyl formate and ammonia gas are further reacted to prepare formamide. The latter is widely used in the industrial field of formamide synthesis at present. However, the process has a series of significant problems which are difficult to break through: (1) the use of carbon monoxide brings about potential safety hazards; (2) sodium formate is used as corrosive strong base, and can damage equipment in the using process; (3) the reaction conditions of high temperature and high pressure have extremely high requirements on equipment (the equipment is high in manufacturing cost and complex in later maintenance and repair), and potential safety hazards exist; (4) the reaction conditions of high temperature and high pressure are extremely energy-consuming, and environmental pollution is caused by the accompanying polluting substances. Not only are these production methods not sustainable on the raw materials, but they also generate large amounts of greenhouse gases which further deteriorate the environment.
Therefore, the development of a green and mild synthesis process for preparing amide compounds is the focus of current research. Recent studies have found that H is generally used in electrochemical synthesis2The O molecule is used as hydrogen source, and can be generated at normal temperature and normal pressure without providing dangerous substances, high temperature and high pressure and other harsh reaction conditions. Meanwhile, in the electrochemical synthesis process, the electron transfer can realize violent oxidation and reduction processes, and strong oxidants and reducing agents are not needed, so that the danger of the reaction is reduced. In addition, the electrosynthesis process can realize small-scale and dispersive operation, and can save a large amount of transportation cost and labor cost. Therefore, the amide compound synthesized by the electrochemical process has great research value and application prospect.
SUMMERY OF THE UTILITY MODEL
The utility model aims to overcome the defects of the prior art and provide a device for synthesizing amide organic micromolecules by electrocatalysis, aiming at synthesizing amide compounds by an electrochemical process.
The technical purpose of the utility model is realized through the following technical scheme.
The utility model provides a device of electro-catalytic synthesis amide organic micromolecule, includes reaction unit, head tank, three electrode system and separation rectifying column, wherein:
the outlet of the raw material tank is connected with the inlet of the reaction device through a pipeline, and a delivery pump is arranged on the pipeline to control the flow velocity and/or flow of the raw materials;
the pH sensor, the temperature sensor and the pressure sensor are respectively connected with the reaction device to monitor the pH, the temperature and the pressure in the reaction device;
arranging an anode assembly, a cathode assembly and a reference electrode assembly in the reaction device, and arranging a membrane assembly between the anode assembly and the cathode assembly; the anode assembly, the cathode assembly and the reference electrode assembly form a three-electrode system and are connected with external electric control equipment arranged outside the reaction device;
a stirring component is arranged in the reaction device; a first outlet of the reaction device is connected with a gas product storage tank through a pipeline;
the second outlet of the reaction device is connected with the separation rectifying tower through a pipeline, the separation rectifying tower is connected with the first collecting tower and the second collecting tower through pipelines so as to realize the rectification separation of reaction substances, the target product amide substances are gathered to the first collecting tower, and the byproducts are gathered to the second collecting tower.
In the technical scheme, the delivery pump is a peristaltic pump.
In the technical scheme, the membrane component is a Nafion membrane component.
In the technical scheme, the external electric control equipment is a potentiostat.
In the technical scheme, the reference electrode assembly is a saturated calomel electrode, a silver-silver chloride electrode or a mercury oxidized mercury electrode.
In the above technical scheme, the anode assembly is a carbon rod or platinum carbon.
In the technical scheme, the cathode assembly is a copper sheet, a copper net, foam copper, a molybdenum sheet, an iron sheet, foam nickel or carbon cloth.
In the above technical scheme, the stirring component is a mechanical stirring paddle or a magnetic stirring device.
In the above technical solution, the stirring member is disposed at a side of the cathode assembly where the product is generated.
In the technical scheme, the separation and rectification tower is connected with the raw material tank, and raw materials which do not participate in the reaction are separated by rectification and directly flow back.
In the technical scheme, inlets are respectively arranged on the reaction devices at the two sides of the cathode and the anode; and a second outlet is arranged on the reaction device at the cathode side.
The technical scheme of the utility model adopt head tank, electrochemical reaction device and separator technical scheme of mutually supporting, use three electrode systems to carry out the constant potential reaction to the raw materials to the synthetic amide class compound of electrochemistry technology has realized the maximize that the raw materials utilized, has greatly reduced material cost.
Drawings
Fig. 1 is the structure diagram of the utility model, wherein 1 is the head tank, 2 is the pH sensor, 3 is temperature sensor, 4 is the anode assembly, 5 is the cathode assembly, 6 is the Nafion membrane module, 7 is the reference electrode subassembly, 8 is the mechanical agitator, 9 is pressure sensor, 10 is the potentiostat, 11 is the gaseous product storage tank, 12 is the separation rectifying column, 13 is the first collection tower, 14 is the second collection tower, 15 is reaction unit, 16 is the dosing pump.
FIG. 2 shows the nuclear magnetic hydrogen spectrum (NMR) of formic acid and sodium nitrite after electrolysis1H) Spectra.
FIG. 3 is a mass spectrum of the gas phase of ethyl acetate extraction after the electrolysis of formic acid and sodium nitrite as reactants in the embodiment of the present invention.
Detailed Description
The following describes the specific technical solution of the present invention in detail with reference to the accompanying drawings.
As shown in the attached figure 1, the utility model discloses a device for electrochemical synthesis of amide organic micromolecules, including reaction unit, head tank, three electrode system and separation rectifying column, wherein:
the outlet of the raw material tank is connected with the inlet of the reaction device through a pipeline, and a delivery pump is arranged on the pipeline to control the flow speed and/or flow of the raw materials;
the pH sensor, the temperature sensor and the pressure sensor are respectively connected with the reaction device to monitor the pH, the temperature and the pressure in the reaction device, the pH sensor and the temperature sensor monitor the pH and the temperature of a liquid environment in the reaction device, and the pressure sensor monitors the pressure in the reaction device, such as hydrogen and oxygen produced along with the reaction, so as to reduce the danger coefficient of the whole device;
arranging an anode assembly, a cathode assembly and a reference electrode assembly in the reaction device, and arranging a Nafion membrane assembly between the anode assembly and the cathode assembly to divide electrolyte in the reaction device into a catholyte area and an anolyte area; the anode assembly, the cathode assembly and the reference electrode assembly form a three-electrode system and are connected with external electric control equipment arranged outside the reaction device, and a potentiostat is selected as the external electric control equipment because the reaction selects a potentiostat reaction; the reference electrode assembly is a saturated calomel electrode, a silver chloride electrode and a mercury oxide electrode, the anode assembly is a carbon rod or platinum carbon (foil carbon), the cathode assembly is a copper sheet, a copper net, a foam copper, a molybdenum sheet, an iron sheet, a foam nickel or carbon cloth, and the reference electrode assembly is used as a catalyst in a constant potential reaction.
A stirring component is arranged in the reaction device to realize the uniform distribution and reaction of each component, a mechanical stirring paddle or a magnetic stirring device is adopted, and the stirring component is preferably arranged on one side of a cathode assembly with a product generated;
the first outlet of the reaction device is connected with a gas product storage tank through a pipeline to collect gas products, such as hydrogen and oxygen produced along with the reaction;
a second outlet of the reaction device is connected with a separation rectifying tower through a pipeline, the separation rectifying tower is connected with a first collecting tower and a second collecting tower through pipelines so as to realize the rectification separation of reaction substances, the target product amide substances are gathered to the first collecting tower, and the byproducts are gathered to the second collecting tower; in order to improve the utilization rate of reactants and reduce the cost of raw materials, the separation and rectification tower is connected with the raw material tank, the target product amide substance is gathered to the first collection tower, the byproduct is gathered to the second collection tower, and simultaneously, the raw materials which do not participate in the reaction are separated by rectification and directly flow back, so that the maximization of the utilization of the raw materials is realized, and the cost of the raw materials is greatly reduced.
A Nafion membrane component (namely a proton exchange membrane) is arranged in a reaction device, electrolyte in the reaction device is divided into a catholyte area and an anolyte area, the interaction of the electrolyte in the two areas is realized, and a target product amide is generated on one side of a cathode (namely a working electrode).
Use the utility model discloses a preparation of formamide is carried out to the device, as follows:
first, 0.1M NaOH aqueous solution is prepared, and formic acid and sodium nitrite are added in such a manner that the concentrations thereof are 100 mM and 200mM, respectively, and the resulting solution is used as an electrolyte, i.e., a raw material solution, and stored in a raw material tank.
Secondly, operating a quantitative conveying pump (such as a peristaltic pump) and setting the flow rate, and conveying the prepared raw material liquid into the reaction devices from inlets of the reaction devices on the two sides of the cathode and the anode simultaneously; at the same time the mechanical stirrer was switched on and the speed was adjusted and set to 600 revolutions per minute.
And thirdly, adopting a three-electrode system-Ag/AgCl as a reference electrode, a carbon rod as a counter electrode (anode), a copper net as a working electrode (cathode), and adopting a potentiostatic method, wherein the working voltage is set to-0.4V vs. RHE to carry out potentiostatic electrolysis reaction for 10800 s.
Fourthly, in the process of constant potential reaction, the numerical values of the sensors are observed in time and correspondingly operated, namely (1) the numerical value of the pressure sensor is increased, which indicates that the generated gas is converged in the reaction device along with the reaction to generate danger, a first outlet of the reaction device is opened, and the gas is introduced into a gas product storage tank through a pipeline; (2) the temperature or pH value sensor changes, and the adjustment is realized by supplementing the raw material liquid by adjusting the set flow rate in the peristaltic pump.
And fifthly, after the reaction is finished, closing a power supply, connecting a second outlet of the reaction device with a separation rectifying tower through a pipeline, connecting the separation rectifying tower with a first collecting tower and a second collecting tower through pipelines so as to realize the rectification and separation of the reaction substances, converging the target product amide substances into the first collecting tower, converging the byproducts into the second collecting tower, and directly flowing back the raw materials which do not participate in the reaction after rectification and separation.
Collect electrolyte to deuterated N, N-Dimethylformamide (DMSO) is the deuteration reagent, carries out the nuclear magnetic hydrogen spectrum test of water peak suppression, and the result shows that the product is the formamide, as shown in the attached figure 2, goes on after using ethyl acetate extraction with electrolyte, and gas chromatography-mass spectrometry (figure 3), the result also shows that the product is the formamide, proves that formic acid is the carbon source, sodium nitrite is the nitrogen source, uses the utility model discloses the device can realize the successful synthesis of formamide.
Adjust different carbon sources, nitrogen sources and process parameters, all can use the utility model discloses the preparation of amide material is realized to the device.
The invention has been described above by way of example, and it should be noted that any simple variants, modifications or other equivalent substitutions by a person skilled in the art without spending creative effort may fall within the scope of protection of the present invention without departing from the core of the present invention.
Claims (10)
1. The device for synthesizing amide organic micromolecules through electrocatalysis is characterized by comprising a reaction device, a raw material tank, a three-electrode system and a separation rectifying tower, wherein:
the outlet of the raw material tank is connected with the inlet of the reaction device through a pipeline, and a delivery pump is arranged on the pipeline to control the flow velocity and/or flow of the raw materials; the pH sensor, the temperature sensor and the pressure sensor are respectively connected with the reaction device to monitor the pH, the temperature and the pressure in the reaction device;
arranging an anode assembly, a cathode assembly and a reference electrode assembly in the reaction device, and arranging a membrane assembly between the anode assembly and the cathode assembly; the anode assembly, the cathode assembly and the reference electrode assembly form a three-electrode system and are connected with external electric control equipment arranged outside the reaction device;
a stirring component is arranged in the reaction device; a first outlet of the reaction device is connected with a gas product storage tank through a pipeline;
the second outlet of the reaction device is connected with the separation rectifying tower through a pipeline, the separation rectifying tower is connected with the first collecting tower and the second collecting tower through pipelines so as to realize the rectification separation of reaction substances, the target product amide substances are gathered to the first collecting tower, and the byproducts are gathered to the second collecting tower.
2. The device for electrocatalytic synthesis of amide-type organic small molecules as claimed in claim 1, wherein the delivery pump is a peristaltic pump.
3. The device for electrocatalytic synthesis of amide organic small molecules as claimed in claim 1, wherein the membrane module is a Nafion membrane module.
4. The device for electrocatalytic synthesis of amide-type organic small molecules according to claim 1, wherein the external electronic control device is a potentiostat.
5. The device for electrocatalytic synthesis of amide organic small molecules as claimed in claim 1, wherein the reference electrode assembly is a saturated calomel electrode, a silver chloride electrode or a mercury oxidized mercury electrode.
6. The device for electrocatalytic synthesis of amide-type organic small molecules as claimed in claim 1, wherein the anode assembly is carbon rod or platinum carbon.
7. The device for electrocatalytic synthesis of amide organic small molecules as claimed in claim 1, wherein the cathode assembly is a copper sheet, a copper mesh, a copper foam, a molybdenum sheet, an iron sheet, a nickel foam or a carbon cloth.
8. The device for electrocatalytic synthesis of amide-type organic small molecules as claimed in claim 1, wherein the stirring component is a mechanical stirring paddle or a magnetic stirring device disposed at the side of the cathode assembly where the product is generated.
9. The device for synthesizing amide organic micromolecules through electrocatalysis as claimed in claim 1, wherein the separation rectification tower is connected with the raw material tank, and raw materials which do not participate in reaction are separated through rectification and directly flow back.
10. The device for electrocatalytic synthesis of amide-type organic small molecules as claimed in claim 1, wherein inlets are respectively disposed on the reaction devices at both sides of the cathode and the anode; and a second outlet is arranged on the reaction device at the cathode side.
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| CN202123066169.1U CN216473513U (en) | 2021-12-08 | 2021-12-08 | Device for synthesizing amide organic micromolecules through electrocatalysis |
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| CN202123066169.1U CN216473513U (en) | 2021-12-08 | 2021-12-08 | Device for synthesizing amide organic micromolecules through electrocatalysis |
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