CN112915966A - Preparation method and application of polyaniline-based activated carbon - Google Patents
Preparation method and application of polyaniline-based activated carbon Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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Abstract
The invention relates to a preparation method and application of polyaniline-based activated carbon. The preparation method of the invention has the advantages of low cost of raw materials, simple process and rich and uniform pores of the prepared active carbon. The polyaniline-based activated carbon prepared by the method can be used as an adsorbent for gas separation, and has good CF4Adsorption capacity and CF4/N2Adsorption selectivity, meets the requirement of CF in industrial production tail gas4And (4) the requirement of trapping.
Description
Technical Field
The invention relates to a preparation method and application of polyaniline-based activated carbon, and relates to the technical field of greenhouse gas emission reduction materials.
Background
Carbon tetrafluoride (CF)4) Is a gas with ultra-high greenhouse effect, which is generated and used in large quantity in the electrolytic aluminum anode and semiconductor etching process. To prevent CF4The air is introduced into the air, and the air is adsorbed and collected by a physical adsorption method. The traditional physical adsorbents such as zeolite, silica gel, alumina and the like have small specific surface area, are easily interfered by water vapor, have poor adsorption effect, and the polyaniline-based activated carbon is greatly researched due to the characteristics of large specific surface area, good hydrophobicity, nitrogen element doping and the like.
In the prior art, there are two main methods for preparing polyaniline-based activated carbon, namely a physical activation method including a water vapor activation method, a carbon dioxide activation method, a mixed gas activation method and the like, and a chemical activation method including a common activator including potassium hydroxide, phosphoric acid, zinc chloride and the like. Although much research is currently done on polyaniline-based activated carbon, most of them are directed to activation conditions and CO2About the application of polyaniline-based activated carbon in CF4The study of adsorption separation is almost nil. With the rapid development of the aluminum industry and the semiconductor industry, CF4Is getting worse and worse, and therefore, a method applicable to CF is sought4Trapped gas adsorbents are increasingly important.
Disclosure of Invention
Technical problem to be solved
In order to solve the above problems of the prior art, the present invention provides a method for preparing polyaniline-based activated carbon, and its application in CF4And (4) trapping the gas.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
a preparation method of polyaniline-based activated carbon comprises the following steps:
s1, raw material synthesis: dissolving aniline in an acid solution, uniformly mixing, slowly adding an oxidant, stirring, filtering, drying and synthesizing polyaniline;
s2, raw material pretreatment: placing the synthesized polyaniline in a horizontal tube furnaceIn, N2Calcining in an atmosphere;
s3, activation: mixing the product obtained in S2 with potassium carbonate powder, grinding into powder, placing into a steel crucible, placing into a horizontal tube furnace, and adding N2Performing secondary calcination in the atmosphere for activation;
s4, washing and drying: and (3) dissolving the product obtained by activation in the S3 in a small amount of water, adding a proper amount of hydrochloric acid solution, stirring, carrying out suction filtration by using a large amount of clear water until the pH value of the filtrate is close to 7, and finally carrying out vacuum drying on the product to obtain the polyaniline-based activated carbon.
In the preparation method described above, preferably, in step S1, the acidic solution is hydrochloric acid, acetic acid or sulfuric acid, and the oxidizing agent is an ammonium persulfate solution.
In the preparation method, preferably, in step S1, the acidic solution is 0.5 to 2mol/L hydrochloric acid, the volume concentration of aniline in the acidic solution is 2 to 5%, the concentration of ammonium persulfate solution is 0.3 to 0.5mol/L, the final concentration of aniline in the acidic solution and the final concentration of ammonium persulfate solution are 1 to 2.25%, the stirring speed is 700 to 800rpm, and the stirring time is 6 to 12 hours; the drying condition is 50-70 ℃, and the drying time is 6-12 h.
In the preparation method, in step S2, the temperature rise rate of the calcination is preferably 3 to 5 ℃/min, the temperature rises to 500 to 600 ℃, and the calcination time is preferably 1.5 to 2.5 hours.
In the preparation method, in step S3, the product obtained in step S2 is preferably mixed with potassium carbonate powder in a mass ratio of 1: 1-4.
Further, the product obtained in step S2 is mixed with potassium carbonate powder in a mass ratio of preferably 1:1 to 2.5.
In the preparation method, in step S3, the temperature rise rate of the secondary calcination is preferably 3 to 5 ℃/min, the temperature of the secondary calcination is preferably 700 to 750 ℃, and the time is preferably 1 to 2 hours.
Further, the temperature of the secondary calcination is most preferably 700 ℃ and the time is 1 h.
In the preparation method, preferably, in step S4, the hydrochloric acid solution has a concentration of 0.5 to 2.5mol/L, and is used to neutralize the residual potassium carbonate powder after the reaction, and the temperature of the vacuum drying is 60 to 80 ℃, and the time is 10 to 12 hours.
The polyaniline-based activated carbon prepared by the preparation method can adsorb CF4Application in gas.
In the above application, preferably, the adsorption condition is that the pressure is 0-1 bar, and the temperature is 0-50 ℃, the adsorption of CF4A gas.
As described above, preferably, the polyaniline-based activated carbon is used for separating CF4And N2CF in mixed gas4。
CF (carbon fiber) prepared by polyaniline-based activated carbon obtained by the preparation method4The application of the adsorbent.
According to a great amount of experimental researches, the ammonium persulfate serving as the oxidant has the final concentration of 0.25mol/L and the final concentration of the added aniline of 1-2.25%, the concentration of the generated polyaniline cannot be increased when the final concentration of the added aniline exceeds 2.25%, the optimal addition amount of the aniline is 1.75% under the condition of certain concentration of the oxidant, the synthesized polyaniline is calcined firstly so as to purify the synthesized polyaniline and remove part of impurities such as tar and the like in the synthesized polyaniline so as not to influence secondary activation, and the calcination temperature is preferably 500-600 ℃. When the secondary calcination temperature is below 600 ℃ for activation, the obtained product is not completely activated, the specific surface area is small, the adsorption capacity is weak, when the secondary calcination temperature is above 800 ℃, the polyaniline part starts to burn without oxygen in the activation process, the product is damaged, and the adsorption capacity is poor, compared with the condition that the secondary calcination temperature is preferably 700-750 ℃, the activation at 700 ℃ is most suitable.
(III) advantageous effects
The invention has the beneficial effects that:
the preparation method of the polyaniline-based activated carbon provided by the invention takes polyaniline and potassium carbonate as raw materials, and has the advantages of low raw material cost, no toxicity, no corrosiveness, environmental friendliness, simple preparation process and low operation difficulty. The polyaniline-based activated carbon prepared can be used as CF4Adsorbent of good CF4/N2Selectivity, CF in the mixed gas4And N2The separation of (2) meets the requirement of CF in the industrial production tail gas4Compared with the prior adsorbent, the adsorbent has better adsorption performance.
The polyaniline-based activated carbon obtained by the preparation method of the polyaniline-based activated carbon provided by the invention has larger specific surface area and pore volume, good chemical stability and water resistance, meanwhile, the polyaniline contains nitrogen, and the derived activated carbon contains a large number of nitrogen functional groups, so that the active sites on the surface are increased, and the polyaniline-based activated carbon is an ideal adsorbent.
Drawings
FIG. 1 is a flow chart of the production process in example 1;
FIG. 2 is an SEM photograph of polyaniline-based activated carbon in example 1;
FIG. 3 is the CF of polyaniline-based activated carbon at 0 deg.C, 25 deg.C and 50 deg.C under different pressures4Adsorption isotherms;
FIG. 4 is a graph showing CF pressures at 25 ℃ and different pressures for the polyaniline-based activated carbon prepared in examples 1 to 44Adsorption isotherms;
FIG. 5 is the CF of polyaniline-based activated carbon at 25 ℃ under different pressures4And N2Adsorption isotherms;
FIG. 6 shows the activated carbon based on polyaniline obtained in example 1 and comparative example vs CF at 25 ℃ under different pressures4Adsorption isotherms;
FIG. 7 shows the comparison of CF at different pressures at 25 ℃ for the prior art adsorbent and the adsorbent prepared by the present invention4Adsorption isotherms.
Detailed Description
For the purpose of better explaining the present invention and to facilitate understanding, the present invention will be described in detail by way of specific embodiments with reference to the accompanying drawings.
Example 1
A preparation method of polyaniline-based activated carbon is detailed in a flow chart of figure 1, and specifically comprises the following steps:
(1) dissolving 7.2mL of aniline in 200mL of 1mol/L hydrochloric acid solution, uniformly mixing, slowly adding 200mL of 0.5mol/L ammonium persulfate solution, stirring at 700rpm for 12h, filtering, and drying at 60 ℃ for 12h to synthesize Polyaniline (PANI);
(2) placing the synthesized polyaniline in a horizontal tube furnace, N2Calcining for 2h at the temperature rising rate of 5 ℃/min to 550 ℃ in the atmosphere;
(3) mixing the product obtained in (2) with potassium carbonate powder in a ratio of 1: 2, grinding into fine powder, placing into a steel crucible, placing into a horizontal tube furnace, and placing into a horizontal tube furnace2Activating in the atmosphere, and calcining for 1h at 700 ℃ according to the heating rate of 5 ℃/min;
(4) and (3) dissolving the intermediate product obtained by activation in the step (3) in water, adding 100mL of 2mol/L hydrochloric acid solution to neutralize potassium carbonate which is not completely activated, stirring, carrying out suction filtration by using a large amount of deionized water until the pH value of the filtrate is close to 7, and finally carrying out vacuum drying on the product at 70 ℃ for 12 hours to obtain the polyaniline-based activated carbon.
Scanning electron microscope detection is carried out on the polyaniline-based activated carbon obtained by preparation to obtain an SEM image as shown in figure 2, and the SEM image shows that a large amount of uniform porous structures exist on the surface of the obtained polyaniline-based activated carbon, and the obtained polyaniline-based activated carbon is smooth and flat in texture.
Example 2
The embodiment provides a preparation method of polyaniline-based activated carbon, which comprises the following steps:
(1) dissolving 7.2mL of aniline in 200mL of 1mol/L hydrochloric acid solution, uniformly mixing, slowly adding 200mL of 0.5mol/L ammonium persulfate solution, stirring at 800rpm for 12h, filtering, and drying;
(2) placing the synthesized polyaniline in a horizontal tube furnace, N2Heating to 550 ℃ in the atmosphere at a heating rate of 5 ℃/min and calcining for 2 h;
(3) mixing the product obtained in (2) with potassium carbonate powder in a ratio of 1:1, grinding into fine powder, placing into a steel crucible, placing into a horizontal tube furnace, and placing into a horizontal tube furnace2In the atmosphere, heating to 700 ℃ at the heating rate of 5 ℃/min, calcining for 1h, and activating;
(4) dissolving the product obtained by activation in the step (3) in water, adding 100mL of 2mol/L hydrochloric acid solution, stirring, carrying out suction filtration by using a large amount of clear water until the pH value of the filtrate is close to 7, and finally carrying out vacuum drying on the product at 70 ℃.
Example 3
The embodiment provides a preparation method of polyaniline-based activated carbon, which comprises the following steps:
(1) dissolving 7.2mL of aniline in 200mL of 1mol/L hydrochloric acid solution, uniformly mixing, slowly adding 200mL of 0.5mol/L ammonium persulfate solution, stirring at 750rpm for 12h, filtering, and drying;
(2) placing the synthesized polyaniline in a horizontal tube furnace, N2Heating to 550 ℃ in the atmosphere at a heating rate of 5 ℃/min and calcining for 2 h;
(3) mixing the product obtained in (2) with potassium carbonate powder in a ratio of 1: 3, grinding into fine powder, placing into a steel crucible, placing into a horizontal tube furnace, and placing into a horizontal tube furnace2In the atmosphere, heating to 700 ℃ at the heating rate of 5 ℃/min, calcining for 1h, and activating;
(4) dissolving the product obtained by the activation in the step (3) in water, adding 80mL of 2mol/L hydrochloric acid solution, stirring, carrying out suction filtration by using a large amount of clear water until the pH value of the filtrate is close to 7, and finally carrying out vacuum drying on the product at 70 ℃.
Example 4
The embodiment provides a preparation method of polyaniline-based activated carbon, which comprises the following steps:
(1) dissolving 7.2mL of aniline in 200mL of 1mol/L hydrochloric acid solution, uniformly mixing, slowly adding 200mL of 0.5mol/L ammonium persulfate solution, stirring at 800rpm for 12h, filtering, and drying;
(2) placing the synthesized polyaniline in a horizontal tube furnace, N2Heating to 550 ℃ in the atmosphere at a heating rate of 5 ℃/min and calcining for 2 h;
(3) mixing the product obtained in (2) with potassium carbonate powder in a ratio of 1: 4, grinding into fine powder, putting the powder into a steel crucible, putting the crucible into a horizontal tube furnace, and putting the crucible into a horizontal tube furnace2Calcining for 1h at 700 ℃ at the heating rate of 5 ℃/min in the atmosphere;
(4) dissolving the product obtained by the activation in the step (3) in water, adding 80mL of 2mol/L hydrochloric acid solution, stirring, carrying out suction filtration by using a large amount of clear water until the pH value of the filtrate is close to 7, and finally carrying out vacuum drying on the product at 70 ℃.
Example 5
In this example, the application of polyaniline-based activated carbon obtained in example 1 was used as an adsorbent, and a JW-BK112 model specific surface area and pore size analyzer from the beijing jinggangbo company was used to test CF at different pressures and different temperatures4Before testing the adsorption capacity of the polyaniline-based activated carbon provided by the invention, the polyaniline-based activated carbon is degassed for 6 hours at 300 ℃ in a vacuum state.
Using physical adsorption instrument at 0 deg.C, 25 deg.C and 50 deg.C for single-component CF4The adsorption experiment of gas was carried out, and an adsorption curve was plotted with pressure as abscissa and adsorption amount as ordinate, as shown in fig. 3, and the results showed that the polyaniline-based activated carbon was responsible for CF at 0 ℃, 25 ℃ and 50 ℃ at 1bar (100kPa)4The amounts of adsorption of (A) were 2.84mmol/g, 2.11mmol/g and 1.49mmol/g, respectively.
The polyaniline-based activated carbon prepared in examples 1 to 4 was degassed at 300 ℃ for 6 hours in a vacuum state, and single-component CF was treated at 25 ℃ using a physical adsorption apparatus4The adsorption experiment of the gas is carried out, an adsorption curve graph is drawn by taking the pressure as the abscissa and the adsorption amount as the ordinate, as shown in fig. 4, the result shows that the best method is adopted in the embodiment 1, the potassium carbonate amount is less and the activation is incomplete in the embodiment 2, and the excessive activation of the raw material, the damaged pore channel and the reduction of the adsorption amount are caused along with the increase of the potassium carbonate amount in the embodiment 3 and the embodiment 4.
Example 6
This example provides the application of polyaniline-based activated carbon prepared in this invention, which is measured at 25 ℃ using the polyaniline-based activated carbon obtained in example 1 as adsorbent, to single-component CF4And N2The adsorption capacity of the polyaniline-based active carbon to CF at 25 DEG C4And N2The adsorption isotherm of (a) is shown in fig. 5. As can be seen from FIG. 5, in the case of 1bar and 25 ℃ adsorption temperature, polyaniline-based activated carbon is present for CF4Has greater adsorption capacity but for N2Has a very small adsorption capacity, i.e. is polymerizedPhenylamine-based activated carbon para-CF4/N2The mixed gas has high adsorption selectivity and can be used for separating CF4/N2CF in the mixed gas4。
Comparative example
On the basis of example 1, it differs from example 1 in that step (3) is not carried out, i.e. the product obtained in step (2) is directly subjected to step (4), the final product is degassed at 300 ℃ under vacuum for 6h, and then the CF of the single component is subjected to a physical adsorption apparatus at 25 ℃ in a single component4The adsorption experiment of the gas is carried out, an adsorption curve graph is drawn by taking the pressure as the abscissa and the adsorption amount as the ordinate, and the figure 6 shows that the polyaniline which is not activated by the potassium carbonate basically has no CF4And (4) gas adsorption.
Commercial activated carbon (purchased from Dakott energy science and technology Co., Ltd., Sichuan), zeolite 13X, zeolite 5A, zeolite 4A (Sigma Aldrich) in the prior art and polyaniline-based activated carbon prepared in the embodiment 1 of the present invention were subjected to a physical adsorption apparatus at 25 ℃ to form a single-component CF4The adsorption experiment is carried out on the gas, the pressure is taken as the abscissa, the adsorption capacity is taken as the ordinate to draw an adsorption curve chart, the result is shown in figure 7, and the figure shows that the polyaniline-based activated carbon prepared by the method has better CF adsorption capacity4The action of the gas.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art can change or modify the technical content disclosed above into an equivalent embodiment with equivalent changes. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (10)
1. A preparation method of polyaniline-based activated carbon is characterized by comprising the following steps:
s1, raw material synthesis: dissolving aniline in an acid solution, uniformly mixing, slowly adding an oxidant, stirring, filtering, drying and synthesizing polyaniline;
s2, raw material pretreatment: placing the synthesized polyaniline in a horizontal tube furnace, N2Calcining in an atmosphere;
s3, activation: mixing the product obtained in S2 with potassium carbonate powder, grinding into powder, placing into a steel crucible, placing into a horizontal tube furnace, and adding N2Performing secondary calcination in the atmosphere for activation;
s4, washing and drying: and (3) dissolving the product obtained by activation in the S3 in a small amount of water, adding a proper amount of hydrochloric acid solution, stirring, carrying out suction filtration by using a large amount of clear water until the pH value of the filtrate is close to 7, and finally carrying out vacuum drying on the product to obtain the polyaniline-based activated carbon.
2. The method of claim 1, wherein in step S1, the acidic solution is hydrochloric acid, sulfuric acid, or acetic acid, and the oxidizing agent is an ammonium persulfate solution.
3. The preparation method according to claim 1, wherein in step S1, the acidic solution is 0.5 to 2mol/L hydrochloric acid, the volume concentration of aniline in the acidic solution is 2 to 5%, the concentration of ammonium persulfate solution is 0.3 to 0.5mol/L, the final concentration of aniline in the acidic solution and the final concentration of ammonium persulfate solution are 1 to 2.25%, the stirring speed is 700 to 800rpm, the stirring time is 6 to 12 hours, and the drying condition is 50 to 70 ℃, and the drying time is 6 to 12 hours.
4. The method of claim 1, wherein in step S2, the temperature rise rate of the calcination is 3-5 ℃/min, the temperature rises to 500-600 ℃, and the calcination time is 1.5-2.5 h.
5. The preparation method of claim 1, wherein in step S3, the product obtained in S2 is mixed with potassium carbonate powder in a mass ratio of 1: 1-4; the temperature rise rate of the secondary calcination is 3-5 ℃/min, the temperature of the secondary calcination is 700-750 ℃, and the time is 1-2 h.
6. The preparation method of claim 1, wherein in step S4, the hydrochloric acid solution has a concentration of 0.5 to 2.5mol/L, and is used to neutralize the residual potassium carbonate powder after the reaction, and the temperature of the vacuum drying is 60 to 80 ℃ and the time is 10 to 12 hours.
7. The polyaniline-based activated carbon obtained by the preparation method as described in any one of claims 1 to 6 adsorbing CF4Application in gas.
8. The use according to claim 7, wherein the adsorption conditions are a pressure of 0 to 1bar and a temperature of 0 to 50 ℃ for adsorbing CF4A gas.
9. Use according to claim 7, wherein the polyaniline-based activated carbon is used for the separation of CF4And N2CF in mixed gas4。
10. Use of polyaniline-based activated carbon obtained by the method according to any one of claims 1 to 6 in the production of CF4The application of the adsorbent.
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