CN115142258B - Efficient preparation method of PAN-based activated carbon fiber felt - Google Patents
Efficient preparation method of PAN-based activated carbon fiber felt Download PDFInfo
- Publication number
- CN115142258B CN115142258B CN202210738013.3A CN202210738013A CN115142258B CN 115142258 B CN115142258 B CN 115142258B CN 202210738013 A CN202210738013 A CN 202210738013A CN 115142258 B CN115142258 B CN 115142258B
- Authority
- CN
- China
- Prior art keywords
- temperature
- felt
- activated carbon
- carbon fiber
- furnace
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M11/73—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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M11/01—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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
The invention discloses a high-efficiency preparation method of PAN-based activated carbon fiber felt, which comprises the following specific steps: 1) Carrying out aftertreatment with the temperature of 270 ℃ and the time of 10min on the pre-oxidized felt in a pre-oxidized furnace; 2) Weighing Na 2 CO 3 And K 2 CO 3 The molar ratio is 0.25-4, and the mixture is put into a sealed muffle furnace after being evenly mixed, and the temperature is increased to 950 ℃ under the air condition to obtain Na-K eutectic; 3) The post-treatment felt is immersed in Na-K eutectic aqueous solution and then dried; 4) And (3) introducing steam 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 water vapor and Na-K eutectic and a one-step activation process, so that the processing difficulty and the preparation cost are greatly reduced.
Description
Technical Field
The invention relates to an activated carbon fiber and a preparation method thereof.
Background
With the development of society and the continuous deepening of industrial processes, environmental pollution problems become increasingly serious. The novel adsorption material of the activated carbon fiber has the opportunity of expanding the body and hands facing the challenges brought by environmental pollution. Compared with the materials such as granular activated carbon, the activated carbon fiber can be applied to more environments because of the tow form of the activated carbon fiber, and meanwhile, the problems of secondary pollution and the like are not caused, but the research on PAN-based activated carbon fiber products is less at present, most students consider that the process for preparing the activated carbon fiber is mature, the performance of the activated carbon fiber can basically meet the social requirement, and the wide market and application prospect of the high-performance activated carbon fiber felt are ignored. Although many researches are carried out on the activated carbon fiber at present, the activated carbon fiber sold in the market is still mainly viscose-based activated carbon fiber, however, the viscose-based activated carbon fiber has lower strength, serious pulverization degree and easy secondary pollution in the use process, and the viscose-based activated carbon fiber is mainly of a micropore structure, so that the activated carbon fiber is difficult to adsorb for some larger molecules, and the application of the activated carbon fiber is greatly restricted. Therefore, the industrial production of the activated carbon fiber is enlarged, and the improvement of the production efficiency of the industrial production and the product performance of the activated carbon fiber and related products thereof is very important work.
At present, the research on the activated carbon fiber is still mainly carried out by using tows, and two main problems exist in the industrial production of the activated carbon fiber: firstly, the continuous production efficiency of the filament bundles is lower, and the industrialized production cost is higher; secondly, in order to ensure the continuity of continuous production of the tows, the problem that the tows cannot break in the production process must be ensured, so that the activation process becomes more complex, and the requirement on activation equipment is high. The development and application of activated carbon fibers 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 compared with the production efficiency of the activated carbon fiber, the production efficiency is improved by times; secondly, the requirements of the activated carbon fiber felt on equipment are not high; thirdly, the source of raw materials of the activated carbon fiber felt is wider, and the used pre-oxidized fiber felt is formed by intertwining pre-oxidized fibers through a physical needling method, so that the requirements on pre-oxidized fibers are lower, and the cost is lower. The invention innovatively utilizes the synergistic activation mechanism of the water vapor and Na-K eutectic to ensure the preparation of the activated felt with high specific surface area through a one-step activation process, and simultaneously greatly reduces the processing difficulty and the preparation cost.
Disclosure of Invention
The invention aims to provide a method for efficiently preparing PAN-based activated carbon fiber felt with high specific surface area by utilizing water vapor and Na-K eutectic coaction activation, which 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 invention adopts the following technical scheme:
a high-efficiency preparation method of PAN-based activated carbon fiber felt comprises the following specific steps:
1) A pre-oxidation furnace with uniform temperature is selected for post-treatment, and the pre-oxidation felt is subjected to treatment with the temperature of 270 ℃ and the time of 10min in the pre-oxidation furnace;
2) Weighing Na 2 CO 3 And K 2 CO 3 Mixing with mortar, placing in a ceramic boat, and mixingHeating to 950 ℃ in a sealed muffle furnace, staying for 30min, cooling to room temperature, taking out, and finally grinding the obtained Na-K eutectic and placing in a constant-temperature drying oven for later use;
3) The post-treatment felt is immersed by Na-K eutectic aqueous solutions with different concentrations and then subjected to a single drying process with the temperature of 200 ℃ and the time of 15 min;
4) And (3) placing the pre-oxidized felt after the impregnation treatment into an activation furnace, introducing protective gas and activation reaction gas, and raising the temperature of different temperature areas to a target temperature by programming to activate the pre-oxidized felt.
In the invention, the Na 2 CO 3 And K 2 CO 3 The weighed molar ratio is 0.25-4.
In the invention, the concentration ranges of the used different Na-K eutectic aqueous solutions are as follows: 0-10%.
In the invention, the protective gas is one or more than two mixed gases selected from 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 the iodine adsorption, the benzene adsorption and the BET measuring instrument so as to characterize the pore structure and the adsorption capacity of the activated carbon fiber felt.
Drawings
Fig. 1 is a process flow diagram of a method for efficiently preparing PAN-based activated carbon fiber felt 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, as shown in a figure I, comprises the following steps:
1) A pre-oxidation furnace with uniform temperature is selected for post-treatment, and the pre-oxidation felt is subjected to treatment with the temperature of 270 ℃ and the time of 10min in the pre-oxidation furnace;
2) Weighing Na 2 CO 3 And K 2 CO 3 The mixture is mixed evenly by using a mortar and then placed in a ceramic boat, and the mixture is heated to 950 ℃ in a sealed muffle furnace for stayingTaking out after cooling to room temperature for 30min, and finally grinding the obtained Na-K eutectic and placing the ground Na-K eutectic in a constant temperature drying oven for later use;
3) The post-treatment felt is immersed by Na-K eutectic aqueous solutions with different concentrations and then subjected to a single drying process with the temperature of 200 ℃ and the time of 15 min;
4) And (3) placing the pre-oxidized felt after the impregnation treatment into an activation furnace, introducing protective gas and activation reaction gas, and raising the temperature of different temperature areas to a target temperature by programming to activate the pre-oxidized felt.
In the embodiment of the present invention, the different na—k eutectic concentrations used in step 3) are: 0-10%.
In the embodiment of the present invention, the protective gas introduced in step 4) is one or more than two mixed gases selected from nitrogen, helium and argon, and the activating gas is water vapor.
In the embodiment of the invention, the target temperature of the programmed temperature 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 subjected to post-treatment in a pre-oxidized furnace at 270 ℃ for 10min is directly subjected to steam activation in a nitrogen atmosphere without being immersed by Na-K eutectic, and the target temperature of the programmed temperature of the activation furnace is 850 ℃.
| Iodine adsorption value (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 mixture is uniformly mixed by using a mortar and then placed in a ceramic boat, the temperature is raised to 950 ℃ in a sealed muffle furnace for 30min, and the mixture is taken out after being cooled to room temperature, so that Na-K eutectic is prepared;
the PAN pre-oxidized felt subjected to post-treatment in a pre-oxidized furnace at 270 ℃ for 10min is immersed in 1% concentration Na-K eutectic aqueous solution, and then is subjected to steam activation in nitrogen atmosphere, and the target temperature of furnace programming temperature is 800 ℃.
| Iodine adsorption value (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 mixture is uniformly mixed by using a mortar and then placed in a ceramic boat, the temperature is raised to 950 ℃ in a sealed muffle furnace for 30min, and the mixture is taken out after being cooled to room temperature, so that Na-K eutectic is prepared;
the PAN pre-oxidized felt subjected to post-treatment in a pre-oxidized furnace at 270 ℃ for 10min is immersed in a 3% concentration Na-K eutectic aqueous solution, and then is subjected to steam activation in a nitrogen atmosphere, wherein the target temperature of furnace programming temperature is 850 ℃.
| Iodine adsorption value (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 The molar ratio is 2, the mixture is uniformly mixed by using a mortar and then placed in a ceramic boat, the temperature is raised to 950 ℃ in a sealed muffle furnace for 30min, and the mixture is taken out after being cooled to room temperature, so that Na-K eutectic is prepared;
the PAN pre-oxidized felt subjected to post-treatment in a pre-oxidized furnace at 270 ℃ for 10min is immersed in a 3% concentration Na-K eutectic aqueous solution, and then is subjected to steam activation in a nitrogen atmosphere, wherein the target temperature of furnace programming temperature is 850 ℃.
| Iodine adsorption value (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 The mixture is uniformly mixed by using a mortar and then placed in a ceramic boat, the mixture is heated to 950 ℃ in a sealed muffle furnace for 30min, cooled to room temperature and taken out to prepare Na-K eutectic;
the PAN pre-oxidized felt subjected to post-treatment in a pre-oxidized furnace at 270 ℃ for 10min is immersed in 4% concentration Na-K eutectic aqueous solution, and then is subjected to steam activation in nitrogen atmosphere, and the target temperature of furnace programming temperature is 850 ℃.
| Iodine adsorption value (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 mixture is uniformly mixed by using a mortar and then placed in a ceramic boat, the mixture is heated to 950 ℃ in a sealed muffle furnace for 30min, cooled to room temperature and taken out to prepare Na-K eutectic;
the PAN pre-oxidized felt subjected to post-treatment in a pre-oxidized furnace at 270 ℃ for 10min is immersed in 5% concentration Na-K eutectic aqueous solution, and then is subjected to steam activation in nitrogen atmosphere, and the target temperature of furnace programming temperature is 900 ℃.
| Iodine adsorption value (mg/g) | Specific surface area (m) 2 /g) | Yield (%) |
| 2231 | 2175 | 14.5 |
Claims (6)
1. The efficient preparation method of the PAN-based activated carbon fiber felt is characterized by comprising the following steps of:
1) A pre-oxidation furnace with uniform temperature is selected for post-treatment, and the pre-oxidation felt is subjected to treatment with the temperature of 270 ℃ and the time of 10min in the pre-oxidation furnace;
2) Weighing Na 2 CO 3 And K 2 CO 3 Uniformly mixing by using a mortar, placing in a ceramic boat, heating to 950 ℃ in a closed muffle furnace, staying for 30min, cooling to room temperature, taking out, and finally grinding the obtained Na-K eutectic and placing in a constant-temperature drying oven for later use;
3) The post-treatment felt is immersed by Na-K eutectic aqueous solutions with different concentrations, and then is subjected to a single drying process with the temperature of 200 ℃ and the time of 15 min;
4) And (3) placing the pre-oxidized felt after the impregnation treatment into an activation furnace, introducing protective gas and activation reaction gas, and raising the temperature of different temperature areas to a target temperature by programming to activate the pre-oxidized felt.
2. As claimed inThe method as claimed in claim 1, wherein the Na is weighed 2 CO 3 And K 2 CO 3 The molar ratio is 0.25 to 4.
3. The method of claim 1, wherein the Na-K eutectic aqueous solution has a concentration of: 0-10%.
4. The method of claim 1, wherein the protective gas is one or more of nitrogen, helium, and argon, and the activating gas is steam.
5. The method of claim 1, wherein the temperature programmed target temperature is: 800-900 ℃.
6. A method for preparing a PAN-based activated carbon fiber felt, which is characterized by being prepared by the method according to any one of claims 1 to 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210738013.3A CN115142258B (en) | 2022-06-24 | 2022-06-24 | Efficient preparation method of PAN-based activated carbon fiber felt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210738013.3A CN115142258B (en) | 2022-06-24 | 2022-06-24 | Efficient preparation method of PAN-based activated carbon fiber felt |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115142258A CN115142258A (en) | 2022-10-04 |
| CN115142258B true CN115142258B (en) | 2023-10-13 |
Family
ID=83407992
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210738013.3A Active CN115142258B (en) | 2022-06-24 | 2022-06-24 | Efficient preparation method of PAN-based activated carbon fiber felt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115142258B (en) |
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 |
-
2022
- 2022-06-24 CN CN202210738013.3A patent/CN115142258B/en active Active
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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115142258A (en) | 2022-10-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20190330061A1 (en) | Honeycomb-like homo-type heterojunction carbon nitride composite material and preparation method thereof, and application in catalytic treatment of waste gas | |
| CN103252214B (en) | Active carbon fiber and graded porous Ni-Ni3P/active carbon fiber composite material as well as preparation and application of two | |
| CN110745825A (en) | Preparation method of high-performance biomass-based shaddock peel oriented activated carbon VOCs adsorbent | |
| CN109110759A (en) | A kind of preparation method of nitrogen, boron codope porous carbon materials | |
| CN108048957A (en) | A kind of preparation process of the activated carbon fiber of hollow structure | |
| CN111118671B (en) | Preparation method of 25k large-tow carbon fiber | |
| CN115142258B (en) | Efficient preparation method of PAN-based activated carbon fiber felt | |
| CN114177884A (en) | Three-dimensional integral fibrous porous carbon material, preparation method and application | |
| CN111389448B (en) | Graded porous g-C for photocatalytic degradation3N4Preparation method of @ wood composite material | |
| CN106185931A (en) | A kind of preparation method of active carbon with high specific surface area | |
| CN113215683B (en) | Plantain core-based spiral active carbon fiber and activation method thereof | |
| CN108793120A (en) | The preparation of the double MOF base porous carbon materials of hydrophobicity | |
| CN106219539A (en) | A kind of preparation method of high-specific surface area hierarchical porous structure activated carbon | |
| CN114602455A (en) | Foaming honeycomb denitration catalyst and production method thereof | |
| CN108221181B (en) | The preparation method of special-shaped silicon carbide fibre felt | |
| CN114160104A (en) | Kiln flue gas CO2Trapping and utilizing coupling material and application thereof | |
| CN108940140B (en) | Method for preparing graphene carbon aerogel composite material | |
| CN113976100A (en) | Low-temperature carbonyl sulfide hydrolysis catalyst and preparation method and application thereof | |
| CN112028073A (en) | Preparation method of biomass charcoal-based material | |
| CN103014916B (en) | A kind of device and method of continuous preparation wide cut functional activity Carbon fibe | |
| CN111943198A (en) | Preparation method of coconut shell carbon molecular sieve with high specific surface area | |
| CN108840346A (en) | A kind of method that vertical microwave reactor prepares vermiculite carbon nano tube compound material | |
| CN112517069B (en) | Photocatalytic active carbon aerogel material and preparation method thereof | |
| CN114671432B (en) | Coal-based high-performance CO 2 Preparation method of activated carbon material for adsorption | |
| CN110013828B (en) | Preparation method of modified activated carbon material for flue gas demercuration |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |