CN115142258A - High-efficiency preparation method of PAN-based activated carbon fiber felt - Google Patents
High-efficiency preparation method of PAN-based activated carbon fiber felt Download PDFInfo
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- CN115142258A CN115142258A CN202210738013.3A CN202210738013A CN115142258A CN 115142258 A CN115142258 A CN 115142258A CN 202210738013 A CN202210738013 A CN 202210738013A CN 115142258 A CN115142258 A CN 115142258A
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- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/76—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon oxides or carbonates
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- D06M11/01—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with hydrogen, water or heavy water; with hydrides of metals or complexes thereof; with boranes, diboranes, silanes, disilanes, phosphines, diphosphines, stibines, distibines, arsines, or diarsines or complexes thereof
- D06M11/05—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with hydrogen, water or heavy water; with hydrides of metals or complexes thereof; with boranes, diboranes, silanes, disilanes, phosphines, diphosphines, stibines, distibines, arsines, or diarsines or complexes thereof with water, e.g. steam; with heavy water
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/34—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxygen, ozone or ozonides
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Abstract
The invention discloses a high-efficiency preparation method of a PAN-based activated carbon fiber felt, which comprises the following specific steps: 1) Carrying out post-treatment on the pre-oxidized felt in a pre-oxidation furnace at the temperature of 270 ℃ for 10 min; 2) Weighing Na 2 CO 3 And K 2 CO 3 The molar ratio is 0.25-4, the mixture is put into a sealed muffle furnace after being uniformly mixed, and the temperature is raised to 950 ℃ under the air condition to obtain Na-K eutectic; 3) Soaking the post-treated felt in Na-K eutectic aqueous solution and drying; 4) And introducing water vapor into the activation furnace for activation. The PAN-based activated carbon fiber felt with high specific surface area is prepared by utilizing a synergistic activation mechanism of a water vapor and Na-K eutectic body and a one-step activation process, so that the processing difficulty is greatly reduced, and the PAN-based activated carbon fiber felt is preparedThe method is as follows.
Description
Technical Field
The invention relates to an active carbon fiber and a preparation method thereof.
Background
With the development of society and the continuous deepening of industrialization process, the problem of environmental pollution becomes increasingly serious. In the face of the challenge brought by environmental pollution, the activated carbon fiber, a novel adsorption material, has the opportunity of developing the body greatly. Compared with materials such as granular activated carbon and the like, the activated carbon fiber can be applied to more environments due to the tow form of the activated carbon fiber, and can not cause the problems of secondary pollution and the like, but the research on PAN-based activated carbon fiber products is less at present, most scholars consider that the process for preparing the activated carbon fiber is mature, the performance of the activated carbon fiber can basically meet the social requirements, and the wide market and application prospect of the high-performance activated carbon fiber felt are neglected. Although active carbon fibers are researched more at present, the active carbon fibers sold in the market still mainly use viscose-based active carbon fibers, but the viscose-based active carbon fibers have lower strength and more serious pulverization degree and are easy to cause secondary pollution in the using process, and the viscose-based active carbon fibers are mainly of a microporous structure, so that large molecules are difficult to adsorb, and the application of the active carbon fibers is greatly restricted by the defect. Therefore, it is very important to expand the industrial production of the activated carbon fiber and to improve the production efficiency of the industrial production and the product performance of the activated carbon fiber and related products.
The current research on activated carbon fibers is mainly based on tows, and two problems mainly exist in the industrial production of activated carbon fibers: firstly, the continuous production efficiency of the tows is low, and the industrial production cost is high; in order to ensure the continuous production of the tows, the problem that the tows cannot be broken in the production process needs to be ensured, so that the activation process becomes more complicated, and the requirement on activation equipment is high. The development and application of the activated carbon fiber are limited by the existence of the problems, however, the activated carbon fiber felt has unique advantages as a felt product: firstly, the production efficiency is higher, and is multiplied compared with the production efficiency of the activated carbon fiber; secondly, the requirement of the activated carbon fiber felt on equipment is not high; thirdly, the raw material source of the activated carbon fiber felt is wide, and the used pre-oxidized felt is formed by entwisting pre-oxidized fibers through a physical needling method, so that the requirements on the pre-oxidized fibers are low, and the cost is low. The invention innovatively utilizes the synergistic activation mechanism of the co-molten body of the water vapor and the Na-K to prepare the activated felt with high specific surface area through a one-step activation process, and greatly reduces the processing difficulty and the preparation cost.
Disclosure of Invention
The invention aims to provide a method for efficiently preparing a PAN-based activated carbon fiber felt with a high specific surface area by synergistic activation of water vapor and Na-K eutectic, and aims to solve the problems of difficult processing and high preparation cost of the activated carbon fiber felt.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a high-efficiency preparation method of a PAN-based activated carbon fiber felt comprises the following specific steps:
1) Selecting a pre-oxidation furnace with uniform temperature to perform post-treatment process, and treating the pre-oxidized felt in the pre-oxidation furnace at 270 ℃ for 10 min;
2) Weighing Na 2 CO 3 And K 2 CO 3 Uniformly mixing the materials by using a mortar, placing the materials in a ceramic boat, heating the materials in a sealed muffle furnace to 950 ℃, staying for 30min, cooling the materials to room temperature, taking out the materials, finally grinding the obtained Na-K eutectic and placing the Na-K eutectic in a constant-temperature drying oven for later use;
3) After the post-treatment felt is soaked by Na-K eutectic aqueous solutions with different concentrations, a separate drying process is carried out for 15min at the temperature of 200 ℃;
4) And (3) putting the pre-oxidized felt after the dipping treatment into an activation furnace, introducing protective gas and activation reaction gas, raising the temperature to a target temperature by different temperature zone programs, and activating the pre-oxidized felt.
In the present invention, the Na is 2 CO 3 And K 2 CO 3 The weight molar ratio is 0.25-4.
In the present invention, different aqueous Na — K eutectic solution concentrations were used: 0 to 10 percent.
In the invention, the introduced protective gas is one or more than two mixed gases of nitrogen, helium and argon, and the activating gas is water vapor. In the invention, the target temperature of the temperature programming of the activation furnace is as follows: 800-900 ℃.
In the invention, the specific surface area of the activated carbon fiber felt is calculated by measuring iodine adsorption, benzene adsorption and a BET (BET) tester so as to represent the pore structure and the adsorption capacity of the activated carbon fiber felt.
Drawings
Fig. 1 is a process flow diagram of a high-efficiency preparation method of a PAN-based activated carbon fiber mat according to the present invention.
Detailed Description
The preparation method of the high-activity carbon fiber felt electrode material provided by the embodiment of the invention comprises the following steps as shown in the figure I:
1) Selecting a pre-oxidation furnace with uniform temperature to perform post-treatment process, and treating the pre-oxidized felt in the pre-oxidation furnace at 270 ℃ for 10 min;
2) Weighing Na 2 CO 3 And K 2 CO 3 The molar ratio is 0.25-4, the mixture is placed in a ceramic boat after being uniformly mixed by a mortar, the mixture is heated to 950 ℃ in a sealed muffle furnace and stays for 30min, the mixture is taken out after being cooled to room temperature, and finally the obtained Na-K eutectic is crushed and placed in a constant temperature drying oven for standby;
3) After the post-treatment felt is soaked by Na-K eutectic aqueous solution with different concentrations, a separate drying process with the temperature of 200 ℃ and the time of 15min is carried out;
4) And (3) putting the pre-oxidized felt after the dipping treatment into an activation furnace, introducing protective gas and activation reaction gas, raising the temperature to a target temperature by different temperature zone programs, and activating the pre-oxidized felt.
In the embodiment of the invention, the different concentrations of the Na-K eutectic used in the step 3) are as follows: 0 to 10 percent.
In the embodiment of the invention, the protective gas introduced in the step 4) is one or a mixture of more than two of nitrogen, helium and argon, and the activating gas is water vapor.
In the embodiment of the invention, the target temperature of the programmed temperature rise of the activation furnace used in the step 4) is 800-900 ℃, and the activation time is 15min. Comparative example:
the PAN pre-oxidized felt after being post-treated for 10min in the pre-oxidation furnace at 270 ℃ is directly subjected to water vapor activation in a nitrogen atmosphere without being impregnated with Na-K eutectic, and the target temperature of the programmed temperature rise of the activation furnace is 850 ℃.
| Iodine adsorption number (mg/g) | Specific surface area (m) 2 /g) | Yield (%) |
| 572 | 440 | 60 |
Example 1:
weighing Na 2 CO 3 And K 2 CO 3 The molar ratio is 0.5, the materials are uniformly mixed by using a mortar and then placed in a ceramic boat, the mixture is heated to 950 ℃ in a sealed muffle furnace and stays for 30min, and the mixture is taken out after being cooled to room temperature to prepare Na-K eutectic;
the PAN pre-oxidized felt after being post-treated for 10min in a pre-oxidation furnace at 270 ℃ is soaked in Na-K eutectic aqueous solution with the concentration of 1 percent, and is activated by water vapor in a nitrogen atmosphere, and the temperature programmed in the furnace is 800 ℃.
| Iodine adsorption number (mg/g) | Specific surface area (m) 2 /g) | Yield (%) |
| 736 | 557 | 24.7 |
Example 2:
weighing Na 2 CO 3 And K 2 CO 3 The molar ratio is 1, the materials are uniformly mixed by using a mortar and then placed in a ceramic boat, the mixture is heated to 950 ℃ in a sealed muffle furnace and stays for 30min, and the mixture is taken out after being cooled to room temperature, so that a Na-K eutectic is prepared;
PAN pre-oxidation felt after being post-treated for 10min at 270 ℃ is soaked in Na-K eutectic aqueous solution with the concentration of 3%, water vapor activation is carried out in nitrogen atmosphere, and the target temperature of furnace temperature programming is 850 ℃.
| Iodine adsorption number (mg/g) | Specific surface area (m) 2 /g) | Yield (%) |
| 1091 | 889 | 20.4 |
Example 3:
weighing Na 2 CO 3 And K 2 CO 3 Uniformly mixing the materials according to the molar ratio of 2 by using a mortar, placing the mixture in a ceramic boat, heating the mixture to 950 ℃ in a closed muffle furnace, standing the mixture for 30min, cooling the mixture to room temperature, and taking the mixture out to prepare a Na-K eutectic;
the PAN pre-oxidized felt after being post-treated for 10min in a pre-oxidation furnace at 270 ℃ is soaked in Na-K eutectic aqueous solution with the concentration of 3 percent, and is activated by water vapor in a nitrogen atmosphere, and the temperature programmed in the furnace is 850 ℃.
| Iodine adsorption number (mg/g) | Specific surface area (m) 2 /g) | Yield (%) |
| 1290 | 1019 | 18.3 |
Example 4:
weighing Na 2 CO 3 And K 2 CO 3 Uniformly mixing the materials according to the molar ratio of 4 by using a mortar, placing the mixture in a ceramic boat, heating the mixture to 950 ℃ in a closed muffle furnace, standing the mixture for 30min, cooling the mixture to room temperature, and taking the mixture out to prepare a Na-K eutectic;
the PAN pre-oxidized felt after being post-treated for 10min in a pre-oxidation furnace at 270 ℃ is soaked in Na-K eutectic aqueous solution with the concentration of 4%, and water vapor activation is carried out in a nitrogen atmosphere, wherein the target temperature of the temperature programming of the furnace is 850 ℃.
| Iodine adsorption number (mg/g) | Specific surface area (m) 2 /g) | Yield (%) |
| 1872 | 1631 | 16.1 |
Example 5:
weighing Na 2 CO 3 And K 2 CO 3 The molar ratio is 4, the materials are uniformly mixed by using a mortar and then placed in a ceramic boat, the mixture is heated to 950 ℃ in a sealed muffle furnace and stays for 30min, and the mixture is taken out after being cooled to room temperature, so that a Na-K eutectic is prepared;
the PAN pre-oxidized felt after being post-treated for 10min in a pre-oxidation furnace at 270 ℃ is soaked in Na-K eutectic aqueous solution with the concentration of 5%, and is activated by water vapor in a nitrogen atmosphere, and the target temperature of the temperature programming of the furnace is 900 ℃.
| Iodine adsorption number (mg/g) | Specific surface area (m) 2 /g) | Yield (%) |
| 2231 | 2175 | 14.5 |
Claims (6)
1. A high-efficiency preparation method of PAN-based activated carbon fiber felt is characterized by comprising the following steps:
1) Selecting a pre-oxidation furnace with uniform temperature to perform post-treatment process, and treating the pre-oxidized felt in the pre-oxidation furnace at 270 ℃ for 10 min;
2) Weighing Na 2 CO 3 And K 2 CO 3 Uniformly mixing the materials by using a mortar, placing the mixture in a ceramic boat, heating the mixture to 950 ℃ in a sealed muffle furnace, standing the mixture for 30min, cooling the mixture to room temperature, taking out the mixture, finally grinding the obtained Na-K eutectic and placing the ground Na-K eutectic in a constant-temperature drying oven for later use;
3) Soaking the post-treated felt by Na-K eutectic aqueous solution with different concentrations, and then performing a separate drying process at the temperature of 200 ℃ for 15 min;
4) And (3) putting the pre-oxidized felt after the dipping treatment into an activation furnace, introducing protective gas and activation reaction gas, raising the temperature to a target temperature by different temperature zone programs, and activating the pre-oxidized felt.
2. The method of claim 1, wherein the weighed Na is 2 CO 3 And K 2 CO 3 The molar ratio is 0.25 to 4.
3. The method of claim 1, wherein the aqueous Na-K eutectic solution has a concentration of: 0 to 10 percent.
4. The method of claim 1, wherein the protective gas is one or more of nitrogen, helium and argon, and the activating gas is water vapor.
5. The method of claim 1, wherein the target temperature for the programmed temperature is: 800-900 ℃.
6. A preparation method of PAN-based active carbon fiber felt is characterized by being prepared by the method 1-5.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5922300A (en) * | 1997-01-23 | 1999-07-13 | Oji Paper Co., Ltd. | Process for producing silicon carbide fibers |
| CN103696232A (en) * | 2013-12-11 | 2014-04-02 | 杨学斌 | Activation technology for producing activated carbon fibers |
| CN106702538A (en) * | 2016-12-08 | 2017-05-24 | 北京化工大学 | Preparation method of high-performance activated carbon fibers |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5922300A (en) * | 1997-01-23 | 1999-07-13 | Oji Paper Co., Ltd. | Process for producing silicon carbide fibers |
| CN103696232A (en) * | 2013-12-11 | 2014-04-02 | 杨学斌 | Activation technology for producing activated carbon fibers |
| CN106702538A (en) * | 2016-12-08 | 2017-05-24 | 北京化工大学 | Preparation method of high-performance activated carbon fibers |
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