CN114590791A - Carbon aerogel preparation device and preparation method thereof - Google Patents
Carbon aerogel preparation device and preparation method thereof Download PDFInfo
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- CN114590791A CN114590791A CN202210152086.4A CN202210152086A CN114590791A CN 114590791 A CN114590791 A CN 114590791A CN 202210152086 A CN202210152086 A CN 202210152086A CN 114590791 A CN114590791 A CN 114590791A
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- C01—INORGANIC CHEMISTRY
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
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Abstract
The invention provides a carbon aerogel preparation device, which comprises a raw material barrel, a stirring device and a heating device, wherein a prepared raw material mixed solution containing at least one phenol compound, formaldehyde, an ionic group raw material and a solvent is stored in the raw material barrel; the combined reaction kettle comprises an electro-catalytic reaction zone and an organic solvent replacement reaction zone, wherein the electro-catalytic reaction zone is positioned on the top layer and is communicated with the raw material barrel through a one-way circulation valve, the organic solvent replacement reaction zone is positioned on the bottom layer, the raw material mixed liquor quantitatively circulates into the combined reaction kettle through the one-way circulation valve, electrode wires distributed in a net shape are arranged in the electro-catalytic reaction zone, and current can be introduced into the raw material mixed liquor through the electrode wires; and the carbonization pyrolysis zone can carry out carbonization decomposition reaction on the carbon xerogel and the carbon aerogel precursor generated by the reaction of the combined reaction kettle to generate the carbon aerogel. The invention discloses equipment for industrially and rapidly preparing carbon aerogel, and provides a foundation for industrial production requirements.
Description
Technical Field
The invention relates to the technical field of aerogel preparation, in particular to a carbon aerogel preparation device and a preparation method thereof.
Background
Carbon aerogel is a carbon material prepared in the late 80 s of the 20 th century, and is a novel light nano-scale porous material. The carbon aerogel is obtained by carbonizing the aerogel at high temperature, and a continuous network structure of the aerogel is maintained. The carbon aerogel prepared by the method has the advantages of low specific surface area, single porosity and poor conductivity, and the prepared carbon aerogel has the advantages of low specific surface area, poor conductivity and limits the wide application of the carbon aerogel to a certain extent.
Meanwhile, the existing aerogel production method mostly adopts organic silicon (tetraethoxysilane, methyl orthosilicate and polysiloxane) as a raw material and adopts a supercritical drying or normal-pressure drying method to prepare the aerogel by combining the existing patent technology and literature reports. The supercritical method can be divided into ethanol supercritical drying and carbon dioxide supercritical extraction drying, both raw materials are organic silicon ester, and the methods have the problems of very expensive raw materials, toxicity, complex process, low safety and the like, and seriously restrict the large-scale production and application of the silicon dioxide aerogel. The method for producing the aerogel by adopting the normal pressure method can adopt water glass as a raw material to prepare the silicon dioxide aerogel, obviously reduces the cost of the raw material and the complexity of equipment, but adopts the water glass to prepare the silicon dioxide aerogel, often with the help of an ion exchange resin, so as to prepare a silicic acid solution, and then adds an alkaline catalyst to make the silicic acid solution into gel. And then repeatedly washing the obtained gel with hot water, and preparing the silicon dioxide aerogel under normal pressure after organic solvent replacement and surface methyl silanization reaction. Patent application publication No. CN102167337A discloses that alkali silicate (sodium silicate, potassium silicate) is used as silicon source, water and ethylene glycol are added for dilution, then inorganic acid is added for full reaction for 1-5 hours, then the pH value is adjusted to 2-4, water or alcohol or the mixture thereof is repeatedly used for washing until the content of sodium ion or potassium ion is below 0.1%, and finally the rapid dehydration drying is carried out at the temperature of 100-400 ℃. The method has the disadvantages of complex operation, long production period and low efficiency, and a large amount of salt-containing wastewater is generated in the preparation process. In addition, after the gel is formed, a solvent replacement mode is adopted, ethanol is added into silica sol to directly prepare the alcogel, and the obtained gel still needs to be soaked in ethanol solutions with different concentrations after the gel is formed. Because the process is alcohol-carrying and chlorine-carrying, the durability of the equipment and the requirement on the inner container of the equipment are very high.
In view of the above, there is a need for an improved manufacturing apparatus and method in the prior art to solve the above problems.
Disclosure of Invention
The invention aims to disclose a carbon aerogel preparation device and a preparation method thereof, and provides equipment for industrially and rapidly preparing carbon aerogel.
In order to achieve the above object, the present invention provides a carbon aerogel preparation apparatus, comprising:
the raw material barrel is used for storing a prepared raw material mixed solution containing at least one phenol series compound, formaldehyde, an ionic group raw material and a solvent, and a stirrer is arranged in the raw material barrel;
the combined reaction kettle comprises an electro-catalytic reaction zone and an organic solvent replacement reaction zone, wherein the electro-catalytic reaction zone is positioned on the top layer and is communicated with the raw material barrel through a one-way circulation valve, the organic solvent replacement reaction zone is positioned on the bottom layer, the raw material mixed liquor quantitatively circulates into the combined reaction kettle through the one-way circulation valve, electrode wires distributed in a net shape are arranged in the electro-catalytic reaction zone, and current can be introduced into the raw material mixed liquor through the electrode wires;
and the carbonization pyrolysis zone can carry out carbonization decomposition reaction on the carbon xerogel and the carbon aerogel precursor generated by the reaction of the combined reaction kettle to generate the carbon aerogel.
As a further improvement of the invention, the carbonization pyrolysis zone comprises a drying chamber and a pyrolysis reaction furnace, a water bath device is arranged in the drying chamber, a heating pipe is arranged at the bottom of the water bath device, and a mounting frame and a stirring mechanism arranged on the mounting frame are also arranged in the drying chamber.
As a further improvement of the invention, the stirring mechanism comprises a control motor, the output end of the control motor is fixedly connected with a stirring shaft, and the outer surface of the stirring shaft is fixedly connected with a stirring blade.
As a further improvement of the invention, an organic solvent supply pipeline is arranged in the organic solvent replacement reaction zone and is connected with an external organic solvent storage tank through the supply pipeline, and the organic solvent storage tank is filled with an anhydrous alcohol solvent or an anhydrous ketone solvent.
As a further improvement of the invention, a circulation loop is also arranged in the combined reaction kettle, and the circulation loop can enable the carbon gel precursor solution generated by the electrocatalysis reaction to carry out catalysis and replacement reaction for multiple times.
The invention also discloses a preparation method of the carbon aerogel preparation device, which comprises the following steps:
s1, mixing at least one phenolic compound, formaldehyde, ionic group raw materials and a solvent in advance to obtain a raw material mixed solution, storing the raw material mixed solution in a raw material barrel, and uniformly stirring the ionic groups in the raw material mixed solution through a stirrer;
s2, pumping the raw material mixed liquid in the raw material barrel into a combined reaction kettle, and superposing the raw material mixed liquid in batches according to a certain component to perform catalysis-gel reaction and displacement reaction to obtain a carbon aerogel precursor and carbon xerogel mixture;
and step S3, filling the mixture obtained in the step S2 into a carbonization pyrolysis zone, and performing a temperature rise process and a heat preservation process under the protection of inert gas to finally obtain the carbon aerogel.
As a further improvement of the present invention, the at least one phenolic series compound comprises at least one of resorcinol and its homologues, catechol and its homologues, phenol and its homologues, bisphenol A and its homologues, mixed cresol and its homologues.
As a further improvement of the invention, the molar ratio of at least one phenolic compound and formaldehyde in the raw material mixed liquor is 0.2-1: 1, and the solid content of the raw material mixed liquor is 10% -60%.
As a further improvement of the present invention, the step of carbonizing the carbon xerogel in the step of S2 comprises: and (3) placing the carbon xerogel in an inert gas environment, and controlling carbonization by temperature programming.
As a further improvement of the present invention, the temperature programming includes: heating to 350-500 ℃ at a heating rate of 1-10 ℃/min, and keeping for 0.5-2 hours; after keeping for 0.5-2 hours, heating to 700-1100 ℃ at the heating rate of 1-10 ℃/min, keeping for 0.5-4 hours, and completing carbonization to obtain the carbon aerogel.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention provides a carbon aerogel preparation device and a preparation method thereof, the preparation device and the preparation method of the carbon aerogel provided by the invention are used for catalyzing a raw material mixed solution under the action of continuous current so as to generate sol-gel reaction, and adding ionic groups into the raw material mixed solution, wherein the ionic groups are used as a heteroatom donor and an electron transmission carrier, so that the efficiency of electrochemically catalyzing the sol-gel reaction is improved, the production rate of a carbon aerogel precursor is improved, the carbon aerogel precursor is subjected to solvent replacement, drying and pyrolytic carbonization to obtain the carbon aerogel, and the heteroatom donor enables the obtained carbon aerogel to have heteroatom doping, namely the preparation method of the carbon aerogel provided by the invention prepares the carbon aerogel according to an electrochemical method, wherein the ionic groups are added into the raw material solution so as to provide the heteroatom doping for the carbon aerogel and simultaneously used as the electron transmission carrier, effectively improves the production rate of the carbon aerogel doped with the heteroatom and provides convenience for industrial production. And the reaction regulation of the electrochemical catalysis sol-gel reaction is easy to control.
(2) The preparation method of the carbon aerogel can be used for industrial mass production of the carbon aerogel, and has high production efficiency and high utilization rate.
Detailed Description
The present invention is described in detail below with reference to various embodiments, but it should be understood that these embodiments are not intended to limit the present invention, and those skilled in the art should be able to make modifications and substitutions on the functions, methods, or structures of these embodiments without departing from the scope of the present invention.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The invention relates to a carbon aerogel preparation device and a specific implementation mode of a preparation method thereof.
A carbon aerogel production apparatus, comprising: the raw material barrel is used for storing a prepared raw material mixed solution containing at least one phenol series compound, formaldehyde, an ionic group raw material and a solvent, and a stirrer is arranged in the raw material barrel; the combined reaction kettle comprises an electro-catalytic reaction zone and an organic solvent replacement reaction zone, wherein the electro-catalytic reaction zone is positioned at the top layer and is communicated with the raw material barrel through a one-way circulation valve, the organic solvent replacement reaction zone is positioned at the bottom layer, the raw material mixed liquor quantitatively circulates into the combined reaction kettle through the one-way circulation valve, electrode wires distributed in a net shape are arranged in the electro-catalytic reaction zone, and current can be introduced into the raw material mixed liquor through the electrode wires; and the carbonization pyrolysis zone can carry out carbonization decomposition reaction on the carbon xerogel and the carbon aerogel precursor generated by the reaction of the combined reaction kettle to generate the carbon aerogel. The carbonization pyrolysis zone comprises a drying chamber and a pyrolysis reaction furnace, a water bath device is arranged inside the drying chamber, a heating pipe is arranged at the bottom of the water bath device, a mounting frame is further arranged inside the drying chamber, and an agitating mechanism is arranged on the mounting frame. The stirring mechanism comprises a control motor, the output end of the control motor is fixedly connected with a stirring shaft, and the outer surface of the stirring shaft is fixedly connected with stirring blades. An organic solvent supply pipeline is arranged in the organic solvent replacement reaction zone and is connected with an external organic solvent storage tank through a supply pipeline, and an anhydrous alcohol solvent or an anhydrous ketone solvent is arranged in the organic solvent storage tank. And a circulation loop is also arranged in the combined reaction kettle, and the circulation loop can enable the carbon gel precursor solution generated by the electrocatalysis reaction to carry out catalysis and replacement reaction for multiple times.
The invention also discloses a preparation method of the carbon aerogel preparation device, which comprises the following steps:
s1, mixing at least one phenol series compound, formaldehyde, ionic group raw materials and a solvent in advance to obtain a raw material mixed solution, storing the raw material mixed solution in a raw material barrel, and uniformly stirring the ionic groups in the raw material mixed solution through a stirrer; s2, pumping the raw material mixed liquid in the raw material barrel into a combined reaction kettle, and superposing the raw material mixed liquid in batches according to a certain component to perform catalysis-gel reaction and displacement reaction to obtain a carbon aerogel precursor and carbon xerogel mixture; and step S3, filling the mixture obtained in the step S2 into a carbonization pyrolysis zone, and performing a temperature rise process and a heat preservation process under the protection of inert gas to finally obtain the carbon aerogel. The at least one phenolic compound comprises at least one of resorcinol and its homologues, catechol and its homologues, phenol and its homologues, bisphenol A and its homologues, and cresol and its homologues. The molar ratio of at least one phenolic compound and formaldehyde in the raw material mixed liquor is 0.2-1: 1, and the solid content of the raw material mixed liquor is 10% -60%. The step of carbonizing the carbon xerogel in the step of S2 includes: and (3) placing the carbon xerogel in an inert gas environment, and controlling carbonization by temperature programming. The temperature programming comprises the following steps: heating to 350-500 ℃ at a heating rate of 1-10 ℃/min, and keeping for 0.5-2 hours; after keeping for 0.5-2 hours, heating to 700-1100 ℃ at the heating rate of 1-10 ℃/min, keeping for 0.5-4 hours, and completing carbonization to obtain the carbon aerogel.
Example 1:
in a 100ml electrolytic cell with an inert electrode, 60g of deionized water was added, then 10g of resorcinol, 14g of formaldehyde, and 4g of guanidine carbonate (chemical formula is C2H10N6H2CO3) were weighed into the electrolytic cell, and after magnetic stirring for 30min, 10mA constant current was continuously applied to the electrolytic cell for 8 hours to obtain a carbon aerogel precursor. Soaking the carbon powder in absolute ethyl alcohol for 8 hours, washing the carbon powder, and drying the carbon powder at 90 ℃ under normal pressure to obtain the carbon xerogel. And placing the carbon xerogel on a quartz boat, heating to 400 ℃ at the heating rate of 10 ℃/min in the nitrogen atmosphere, keeping for 0.5h, continuously heating to 1000 ℃ at the heating rate of 6 ℃/min, keeping for 2h, cooling to room temperature, and taking out. The specific surface area of the carbon aerogel sample is 960m2G, density 0.46g/cm3The mesoporous aperture is 4nm, and the content of doping element nitrogen is 2 percent.
The invention discloses a carbon aerogel preparation device and a preparation method thereof, the preparation device and the preparation method of the carbon aerogel provided by the invention are used for catalyzing raw material mixed liquor under the action of continuous current so as to generate sol-gel reaction, and adding ionic groups into the raw material mixed liquor, wherein the ionic groups are used as a heteroatom donor and an electron transmission carrier, so that the efficiency of electrochemically catalyzing the sol-gel reaction is improved, the production rate of a carbon aerogel precursor is improved, the carbon aerogel precursor is subjected to solvent replacement, drying and pyrolytic carbonization to obtain the carbon aerogel, and the heteroatom donor enables the obtained carbon aerogel to have heteroatom doping, namely the preparation method of the carbon aerogel provided by the invention prepares the carbon aerogel according to an electrochemical method, wherein the ionic groups are added into the raw material solution so as to provide heteroatom doping for the carbon aerogel and simultaneously used as the electron transmission carrier, effectively improves the production rate of the carbon aerogel doped with the heteroatom and provides convenience for industrial production. And the reaction regulation of the electrochemical catalysis sol-gel reaction is easy to control. The preparation method of the carbon aerogel can be used for industrial mass production of the carbon aerogel, and has high production efficiency and high utilization rate.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. A carbon aerogel preparation apparatus, comprising:
the raw material barrel is used for storing a prepared raw material mixed solution containing at least one phenol series compound, formaldehyde, an ionic group raw material and a solvent, and a stirrer is arranged in the raw material barrel;
the combined reaction kettle comprises an electro-catalytic reaction zone and an organic solvent replacement reaction zone, wherein the electro-catalytic reaction zone is positioned on the top layer and is communicated with the raw material barrel through a one-way circulation valve, the organic solvent replacement reaction zone is positioned on the bottom layer, the raw material mixed liquor quantitatively circulates into the combined reaction kettle through the one-way circulation valve, electrode wires distributed in a net shape are arranged in the electro-catalytic reaction zone, and current can be introduced into the raw material mixed liquor through the electrode wires;
and the carbonization pyrolysis zone can carry out carbonization decomposition reaction on the carbon xerogel and the carbon aerogel precursor generated by the reaction of the combined reaction kettle to generate the carbon aerogel.
2. The carbon aerogel preparation device of claim 1, wherein the carbonization pyrolysis zone comprises a drying chamber and a pyrolysis reaction furnace, a water bath device is arranged inside the drying chamber, a heating pipe is arranged at the bottom of the water bath device, a mounting frame is further arranged inside the drying chamber, and a stirring mechanism is arranged on the mounting frame.
3. The carbon aerogel preparation device of claim 2, wherein said stirring mechanism comprises a control motor, an output end of said control motor is fixedly connected with a stirring shaft, and an outer surface of said stirring shaft is fixedly connected with a stirring blade.
4. The apparatus of claim 1, wherein said organic solvent replacement reaction zone comprises an organic solvent supply line connected to an external organic solvent storage tank via said supply line, and said organic solvent storage tank contains an anhydrous alcohol solvent or an anhydrous ketone solvent.
5. The apparatus of claim 4, wherein a circulation loop is further provided in the combined reactor, the circulation loop being capable of allowing the carbon gel precursor solution generated by the electrocatalytic reaction to undergo catalytic and displacement reactions for a plurality of times.
6. The method of manufacturing a carbon aerogel manufacturing apparatus of claim 1, comprising the steps of:
s1, mixing at least one phenolic compound, formaldehyde, ionic group raw materials and a solvent in advance to obtain a raw material mixed solution, storing the raw material mixed solution in a raw material barrel, and uniformly stirring the ionic groups in the raw material mixed solution through a stirrer;
s2, pumping the raw material mixed liquid in the raw material barrel into a combined reaction kettle, and superposing the raw material mixed liquid in batches according to a certain component to perform catalysis-gel reaction and displacement reaction to obtain a carbon aerogel precursor and carbon xerogel mixture;
and step S3, filling the mixture obtained in the step S2 into a carbonization pyrolysis zone, and performing a temperature rise process and a heat preservation process under the protection of inert gas to finally obtain the carbon aerogel.
7. The method of manufacturing an apparatus for manufacturing a carbon aerogel according to claim 6, wherein said at least one phenol-series compound comprises at least one of resorcinol and its homologues, catechol and its homologues, phenol and its homologues, bisphenol A and its homologues, and cresol and its homologues.
8. The method of claim 6, wherein the raw material mixture comprises at least one phenol compound and formaldehyde in a molar ratio of 0.2-1: 1, and the raw material mixture has a solid content of 10-60%.
9. The method for producing an apparatus for producing a carbon aerogel according to claim 6, wherein the step of carbonizing said carbon xerogel in the step of S2 comprises: and (3) placing the carbon xerogel in an inert gas environment, and controlling carbonization by temperature programming.
10. The method of manufacturing an apparatus for manufacturing carbon aerogel according to claim 6, wherein said temperature programming comprises: heating to 350-500 ℃ at a heating rate of 1-10 ℃/min, and keeping for 0.5-2 hours; after keeping for 0.5-2 hours, heating to 700-1100 ℃ at the heating rate of 1-10 ℃/min, keeping for 0.5-4 hours, and completing carbonization to obtain the carbon aerogel.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210152086.4A CN114590791A (en) | 2022-02-18 | 2022-02-18 | Carbon aerogel preparation device and preparation method thereof |
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| CN202210152086.4A CN114590791A (en) | 2022-02-18 | 2022-02-18 | Carbon aerogel preparation device and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115395026A (en) * | 2022-08-12 | 2022-11-25 | 陕西科技大学 | Fe monatomic-loaded N-doped carbon aerogel electrocatalyst and preparation method and application thereof |
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2022
- 2022-02-18 CN CN202210152086.4A patent/CN114590791A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115395026A (en) * | 2022-08-12 | 2022-11-25 | 陕西科技大学 | Fe monatomic-loaded N-doped carbon aerogel electrocatalyst and preparation method and application thereof |
| CN115395026B (en) * | 2022-08-12 | 2024-03-15 | 天津市顺红洋科技有限公司 | Fe single-atom-supported N-doped carbon aerogel electrocatalyst and preparation method and application thereof |
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Application publication date: 20220607 |