CN111286773A - Preparation method for enhancing adsorption performance of graphite felt material by electrochemical anodic oxidation - Google Patents
Preparation method for enhancing adsorption performance of graphite felt material by electrochemical anodic oxidation Download PDFInfo
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- CN111286773A CN111286773A CN202010106128.1A CN202010106128A CN111286773A CN 111286773 A CN111286773 A CN 111286773A CN 202010106128 A CN202010106128 A CN 202010106128A CN 111286773 A CN111286773 A CN 111286773A
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- graphite felt
- anodic oxidation
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- deionized water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
Abstract
The invention provides a preparation method for enhancing the adsorption performance of a graphite felt material by electrochemical anodic oxidation; the method comprises the following steps of 1: adjusting the pH value range of the deionized water, adding sodium salt as supporting electrolyte, preparing 500ml of electrolyte, and uniformly stirring for later use; step 2: cutting a graphite felt into a certain size, adding deionized water into an ultrasonic cleaning machine, and cleaning to remove surface impurities; and step 3: and (3) taking the graphite felt as an anode, taking a stone grinding rod as a cathode, taking the solution prepared in the step (1) as an electrolyte, fixing an electrode plate, and electrolyzing under a specified voltage to obtain the graphite felt adsorbing material. The preparation method is simple, has low requirements on equipment, and can remarkably improve the specific surface area and the pore volume of the graphite felt, thereby improving the adsorption removal of pollutants in water. The method has certain universality: in the electrochemical system formed by taking the graphite felt as the anode, after the graphite felt electrode loses the catalytic performance, the graphite felt can be used as an adsorbent, so that the aim of treating wastes with processes of wastes against one another is fulfilled.
Description
Technical Field
The invention relates to the technical field of an electrochemical anodic oxidation modified carbon fiber material; in particular to a preparation method for enhancing the adsorption performance of a graphite felt material by electrochemical anodic oxidation.
Background
The graphite felt is used as a carbon fiber material and has wide application in the fields of electric analysis, electric synthesis, electrochemical advanced oxidation, redox flow batteries, fuel cells and the like. However, graphite felt has relatively few applications for adsorption compared to other carbon fiber materials, such as activated carbon fibers. This is because the graphite felt has a relatively weak adsorption capacity compared to other carbon fiber materials.
The adsorption performance of the carbon material can be enhanced by modification. Common modification methods include surface oxidation/surface reduction modification, metal-loaded modification or chemical vapor deposition. The modification methods are complex in process and long in time consumption, so that the invention of a simple and effective preparation method for enhancing the adsorption performance of the graphite felt is of great significance.
Disclosure of Invention
The invention aims to provide a preparation method for enhancing the adsorption performance of a graphite felt material by electrochemical anodic oxidation.
The invention is realized by the following technical scheme:
the invention relates to a preparation method for enhancing the adsorption performance of a graphite felt material by electrochemical anodic oxidation, which comprises the following steps:
step one, adjusting the numerical range of the pH value of deionized water, adding sodium salt as supporting electrolyte, preparing 500ml of electrolyte (the mass concentration is 1.5g/L), and uniformly stirring for later use;
cutting the graphite felt into a certain size, adding deionized water into an ultrasonic cleaning machine, and cleaning to remove surface impurities;
and step three, taking the graphite felt as an anode, taking a stone grinding rod as a cathode, taking the solution prepared in the step one as electrolyte, fixing an electrode plate, and electrolyzing under a specified voltage by a voltage-stabilizing and current-stabilizing power supply to obtain the graphite felt adsorbing material.
Preferably, in the first step, the adjusting the pH value of the deionized water specifically is: adjusting the pH value of the deionized water to 0-14 by using concentrated sulfuric acid and sodium hydroxide.
Preferably, in the first step, the concentrated sulfuric acid and sodium hydroxide are used for adjusting the pH value of the deionized water, and a supporting electrolyte is added into the solution.
Preferably, in step one, the sodium salt is added in an amount of 0.1 to 2 g.
Preferably, in the second step, the graphite felt has the following dimensions: the length, width and thickness are 6cm, 1.5cm, 0.5 cm.
Preferably, in the second step, the washing time is 20 min.
Preferably, in the third step, the distance between the electrode plates is 4-6 cm.
Preferably, in the third step, the electrolysis time is 0.3-1 h.
Preferably, in the third step, the graphite felt is used as an anode, and the graphite felt of the anode is used as an adsorption material.
The method of the invention has the following advantages:
(1) the preparation method is simple, has low requirements on equipment, and can remarkably improve the specific surface area and the pore volume of the graphite felt, thereby improving the adsorption removal of pollutants in water.
(2) The method has certain universality: in the electrochemical system formed by taking the graphite felt as the anode, after the graphite felt electrode loses the catalytic performance, the graphite felt can be used as an adsorbent, so that the aim of treating wastes with processes of wastes against one another is fulfilled.
Drawings
FIG. 1a is an electron microscope effect diagram of an original graphite felt, and b is a scanning electron microscope effect diagram of the graphite felt obtained by the method of the present invention;
FIG. 2 is a graph showing the pore size distribution of a graphite felt material before and after the application of the present invention;
FIG. 3 is a graph showing the comparison of the decolorization ratio of methylene blue solution with graphite felt as an adsorbing material before and after the application of the present invention;
fig. 4 is a comparison graph of decolorization ratio of methylene blue electrochemically oxidized by using graphite felt as an anode of an electrochemical advanced oxidation system and repeated to 90 times.
Detailed Description
The present invention will be described in detail with reference to specific examples. It should be noted that the following examples are only illustrative of the present invention, but the scope of the present invention is not limited to the following examples.
Examples
The embodiment relates to a preparation method for enhancing the adsorption performance of a graphite felt material by electrochemical anodic oxidation, which comprises the following steps:
step one, adjusting the numerical range of the pH value of deionized water, adding sodium salt as supporting electrolyte, preparing 500ml of electrolyte, and uniformly stirring for later use;
cutting the graphite felt into a certain size, adding deionized water into an ultrasonic cleaning machine, and cleaning to remove surface impurities;
and step three, taking the graphite felt as an anode, taking a stone grinding rod as a cathode, taking the solution prepared in the step one as electrolyte, fixing an electrode plate, and electrolyzing under a specified voltage by a voltage-stabilizing and current-stabilizing power supply to obtain the graphite felt adsorbing material.
The method comprises the following specific steps:
cutting the graphite felt to be 6cm multiplied by 1.5cm multiplied by 0.5cm in length multiplied by width multiplied by thickness, and adding deionized water in an ultrasonic cleaning machine for cleaning for 20min to remove surface impurities for pretreatment.
Then Na with the mass concentration of 1.5g/L is prepared2SO4500ml of electrolyte, using H2SO4Adjusting the pH value of the electrolyte and NaOH to 7.0, uniformly stirring by using a glass cup, taking the pretreated graphite felt as an anode, taking a stone grinding rod as a cathode, fixing the distance between polar plates to be 6cm, and electrolyzing for 40min at a voltage of 7V by using a voltage-stabilizing and current-stabilizing power supply to obtain the prepared graphite felt adsorbing material.
And (3) product effect determination and analysis:
the scanning electron microscope effect of the graphite felt obtained in the embodiment is shown in figure 1 b; the electron microscopy effect of the pristine graphite felt is shown in figure 1 a.
By comparing the two effects, it can be seen that the surface attachments of the graphite felt material obtained in the embodiment are obviously increased, and the surface etching is more, which increases the specific surface area of the material. FIG. 2 is a graph showing pore size distribution of a graphite felt material obtained by BET test before and after the application of the present invention. The test result shows that compared with the original graphite felt, the graphite felt material of the embodiment has greatly increased pore diameter of 2-4nm and specific surface area of 16.14m2The volume/g is increased to 27.84m2/g，VtotalFrom 0.03m3The volume/g is increased to 0.04m3/g。
The graphite felt material obtained in this example was used as an adsorbent and put into 250ml of methylene blue solution with a concentration of 20mg/L to perform an adsorption experiment, the control group was the original graphite felt, and the decolorization rate of methylene blue was shown in fig. 3. The methylene blue decolorization rate of the examples reached 84.02% in 30min, while the methylene blue decolorization rate of the original graphite felt was only 26.17%.
In order to prove the universality of the method, the graphite felt is used as an anode of an electrochemical advanced oxidation system to carry out electrochemical oxidation on methylene blue and is repeated for 90 times, and the electrolyte and the adsorption solution are both 500 ml. The results are shown in FIG. 4. It can be seen that the adsorption decoloring rate of the graphite felt before being used as an anode is very low, only 3.26%, and the decoloring rate of the methylene blue reaches 96.43% when the graphite felt is used as the anode for carrying out electrochemical oxidation on the methylene blue for the first time. After 90 times of repeated use, the electrochemical oxidation performance of the graphite felt as an anode is reduced, and the methylene blue decolorization rate is changed to 71.35%. However, the graphite felt anode after 90 times of repeated use is independently used as an adsorbent to adsorb methylene blue, and the methylene blue decolorization rate is greatly increased to 38.91%. Therefore, the method for enhancing the adsorption performance of the graphite felt through electrochemical anodic oxidation has universality, and the graphite felt anode which loses the electrocatalytic performance after being used as the anode can be used as an adsorbent, so that the aim of treating waste by waste is fulfilled.
The method of the invention has the following advantages:
(1) the preparation method is simple, has low requirements on equipment, and can remarkably improve the specific surface area and the pore volume of the graphite felt, thereby improving the adsorption removal of pollutants in water.
(2) The method has certain universality: in the electrochemical system formed by taking the graphite felt as the anode, after the graphite felt electrode loses the catalytic performance, the graphite felt can be used as an adsorbent, so that the aim of treating wastes with processes of wastes against one another is fulfilled.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (9)
1. A preparation method for enhancing the adsorption performance of a graphite felt material by electrochemical anodic oxidation is characterized by comprising the following steps:
step one, adjusting the numerical range of the pH value of deionized water, adding sodium salt as supporting electrolyte, preparing 500ml of electrolyte, and uniformly stirring for later use;
cutting the graphite felt into a certain size, adding deionized water into an ultrasonic cleaning machine, and cleaning to remove surface impurities;
and step three, taking the graphite felt as an anode, taking a stone grinding rod as a cathode, taking the solution prepared in the step one as electrolyte, fixing an electrode plate, and electrolyzing under a specified voltage by a voltage-stabilizing and current-stabilizing power supply to obtain the graphite felt adsorbing material.
2. The method for preparing graphite felt material with enhanced adsorption property by electrochemical anodic oxidation according to claim 1, wherein in the first step, the adjusting of the pH value of deionized water specifically comprises: adjusting the pH value of the deionized water to 0-14 by using concentrated sulfuric acid and sodium hydroxide.
3. The method of claim 2, wherein in step one, the concentrated sulfuric acid and sodium hydroxide are used to adjust the pH of the deionized water, and a supporting electrolyte is added to the solution.
4. The method of claim 1, wherein in step one, the sodium salt is added in an amount of 0.1-2 g.
5. The method for preparing graphite felt material with enhanced adsorption property by electrochemical anodic oxidation according to claim 1, wherein in the second step, the size of the graphite felt is as follows: the length, width and thickness are 6cm, 1.5cm, 0.5 cm.
6. The method for preparing graphite felt material with enhanced adsorption property by electrochemical anodic oxidation according to claim 1, wherein in the second step, the cleaning time is 20 min.
7. The method for preparing graphite felt material with enhanced adsorption property by electrochemical anodic oxidation according to claim 1, wherein in step three, the distance between the electrode plates is 4-6 cm.
8. The method for preparing graphite felt material with enhanced adsorption property by electrochemical anodic oxidation according to claim 1, wherein in step three, the electrolysis time is 0.3-1 h.
9. The method for preparing graphite felt material with enhanced adsorption property by electrochemical anodic oxidation according to claim 1, wherein in the third step, the graphite felt is used as an anode, and the graphite felt of the anode is used as an adsorption material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111740127A (en) * | 2020-07-03 | 2020-10-02 | 朱义奎 | Electrochemical modification method of graphite felt electrode material of vanadium battery |
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Application publication date: 20200616 |