CN112619599B - Active carbon fiber and preparation method thereof - Google Patents
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- 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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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28011—Other properties, e.g. density, crush strength
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
Abstract
The application provides an activated carbon fiber and a preparation method thereof. The ash content of the activated carbon fiber is 0.8wt% -3wt%, and the specific surface area is 1000m 2 /g‑2200m 2 The total pore volume is 0.4120cc/g-0.8370cc/g, the 1-2nm pore volume ratio is 28% -75%,200mg/m 3 The xylene adsorption capacity is 20-45%. The preparation method of the activated carbon fiber comprises the following steps: impregnating the raw material with a phosphoric acid aqueous solution, drying, carbonizing, cooling, washing and drying to obtain the activated carbon fiber; the mass fraction of the phosphoric acid aqueous solution is 5-13%. According to the activated carbon fiber and the preparation method thereof, phosphoric acid can repeatedly permeate into the fiber, the adhesion phenomenon cannot occur, the production process is continuously carried out, the production efficiency is high, the production cost is low, and the performance of the obtained activated carbon fiber is excellent.
Description
Technical Field
The invention relates to the field of activated carbon fibers, in particular to an activated carbon fiber and a preparation method thereof.
Background
The prior art generally adopts a method of phosphate catalysis and high-temperature carbonization when manufacturing the activated carbon fiber. This method has the following problems: first, the phosphate remaining on the fiber surface causes an increase in product ash; secondly, the phosphate decomposed at high temperature causes great corrosion damage to equipment, and the maintenance cost of the equipment is high, so that the production cost is increased; thirdly, an activator is usually needed to be used, but the activator can cause carbon ablation, greatly reduces the yield of the product (generally only 18-23%), causes great waste of raw materials and further increases the production cost;fourthly, the ablation in the activation stage causes great loss of the carbon material (the loss amount is 30 to 50 percent of the carbonized fiber), so that the activated carbon fiber has a loose structure and the apparent density is generally 60 to 150Kg/m 3 The use of this type of activated carbon fiber is not conducive to the fabrication of miniaturized filter devices. In addition, due to the large ablation of the carbon material, the strength of the activated carbon fiber is poor, so that the service life of a gas filter component made of the activated carbon fiber is reduced; fifthly, the product has small aperture, the proportion of the aperture smaller than 1nm is high, the aperture distribution range is narrow, and the regeneration effect of the activated carbon fiber after adsorption is poor.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the present invention is to provide an activated carbon fiber which has a large specific surface area, high strength, no adhesion problems, a low ash content, and excellent adsorption and desorption properties.
The second purpose of the invention is to provide a preparation method of the activated carbon fiber, which has low cost, high product yield and excellent performance.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the ash content of the activated carbon fiber is 0.8-3 wt%, and the specific surface area is 1000m 2 /g-2200m 2 Per g, the total pore volume is 0.4120cc/g-0.8370cc/g, the 1-2nm pore volume ratio is 28% -75%,200mg/m 3 The xylene adsorption capacity is 20-45%.
A method for preparing activated carbon fibers, comprising:
impregnating the raw material with a phosphoric acid aqueous solution, drying, carbonizing, cooling, washing and drying to obtain the activated carbon fiber;
the raw materials are artificial fibers and/or natural fibers;
the mass fraction of the phosphoric acid aqueous solution is 5-13%.
The use of phosphoric acid as the impregnating solution has the following advantages: 1. the dipping process can be effectively improved, and phosphoric acid can fully permeate into the fibers in the dipping process by controlling the concentration of the phosphoric acid aqueous solution, so that the catalytic dehydration effect of the phosphoric acid can be fully exerted; 2. the generation of tar is inhibited, so that more carbon materials are reserved, and the yield of the final product is improved; 3. the phosphoric acid also has swelling function, and can permeate into the fiber under the condition of lower than 200 ℃ to dissolve the cellulose so as to form a gap; 4. the carbonization is accelerated, the pyrolysis process of the raw material is changed, the activation temperature is reduced, the temperature of the fiber product impregnated with the superphosphoric acid is quickly and uniformly increased, and the local overheating is avoided, so the activation time is short; 5. pore-forming, after phosphoric acid is removed by washing, the original phosphoric acid sites generate corresponding pores; 6. aromatization is promoted, after phosphoric acid is loaded, the size of the polycyclic aromatic hydrocarbon of the fiber raw material is obviously increased, the dehydrogenation temperature is reduced, and the dehydrogenation amount is increased; 7. hydroxyl in phosphoric acid and a polymer are dehydrated and crosslinked, a phosphoric ester bond is generated, the thermal dimensional stability of the cellulose is improved, so that formed pores are reserved, the phosphoric ester bond is destroyed after the temperature is increased, the pores are shrunk, the specific surface and the pore volume are reduced, and then the temperature is continuously increased to ensure that phosphorus oxide produced by decomposing phosphoric acid has oxidizing capacity, so that the pores are continuously improved.
It should be noted that, the phosphoric acid concentration is too low to exert effective action, and the amount of the phosphoric acid solution used is too large, so that the drying time is increased, which is not favorable for continuous production, and meanwhile, the energy consumption is increased and the cost is increased; the concentration of phosphoric acid is too high, so that phosphoric acid cannot repeatedly permeate into the fiber in the dipping process, the problem of serious filament adhesion of the activated carbon fiber can be caused, and the final activated carbon fiber has high brittleness and serious powder removal; in addition, the corrosivity to equipment is increased, the water consumption in the activated carbon fiber washing process is increased, and the energy consumption and the difficulty in the phosphoric acid concentration and recycling process are increased. Therefore, the consumption of the activated carbon fiber in the processes of washing and refining the recovered phosphoric acid can be reduced by using phosphoric acid with proper concentration in the impregnation stage, and the production cost is reduced.
Preferably, the raw material is paper, felt or cloth processed by artificial fiber and/or natural fiber and the respective raw material, and the artificial fiber comprises one or more of viscose fiber, solvent-process cellulose fiber and cuprammonium fiber; the natural fiber comprises one or more of hemp fiber, cotton fiber and silk fiber.
By adopting the raw materials with various forms, products with various forms can be obtained, and the aim of batch production is effectively fulfilled.
Preferably, the mass ratio of the phosphoric acid in the phosphoric acid aqueous solution to the raw material is 0.2-0.8.
Preferably, the dipping time is 10-600min, and the dipping temperature is 10-65 ℃, preferably 40-65 ℃; after the impregnation is finished, the mass ratio of the raw materials to the phosphoric acid to the water is 1: (0.2-0.8): (1.8-9.2).
The impregnation process can be further optimized by controlling the impregnation ratio, the impregnation time and the impregnation temperature. The proportion of the materials after the impregnation is finished can be controlled, so that the impregnation degree can be controlled.
Preferably, the drying mode is airing or hot air drying, the temperature of the drying air is 20-50 ℃, and the mass ratio of the artificial fiber or the natural fiber, the phosphoric acid and the water is 1: (0.2-0.8): (0-1).
Preferably, the carbonization is performed in an air atmosphere or an inert gas atmosphere by a gradient temperature raising method:
the temperature of the first gradient is 50-80 ℃, and the time is 10-30min; the temperature of the second gradient is 90-110 ℃, and the time is 15-32min; the temperature of the third gradient is 120-160 ℃, and the time is 15-40min; the temperature of the fourth gradient is 200-250 ℃ and the time is 10-20min; the temperature of the fifth gradient is 280-300 ℃, and the time is 0-20min; the temperature of the sixth gradient is 300-450 ℃ and the time is 10-90min.
The carbonization process can be optimized by gradient temperature rise, and the carbonization effect is ensured. The gradient temperature rise can lead the heating equipment to work intermittently, generally only accounts for about 30 percent of the total power, the power consumption per hour is greatly reduced, the energy consumption is saved, and the cost is reduced.
Preferably, the end point of the cooling is room temperature.
Preferably, the water washing adopts a multi-stage countercurrent water washing mode, the water washing temperature is 65-95 ℃, and the mass of water used for water washing is 1-12 times of that of the activated carbon fiber; the number of stages is 3-5, and the retention time of each stage of water washing is 5-20min.
Multistage countercurrent water washing can effectively clean the carbonized fiber, reduce ash content and ensure specific surface area.
Optionally, the temperature of the drying is 90-120 ℃; preferably, the drying is carried out by blowing, and the circulation amount of hot air is 300-900m 3 The activated carbon fiber is/kg.
An activated carbon fiber, which is prepared by the preparation method of the activated carbon fiber.
Compared with the prior art, the invention has the following beneficial effects:
(1) The activated carbon fiber provided by the application has the advantages of large specific surface area, low ash content, high strength and good adsorption and desorption properties;
(2) The preparation method of the activated carbon fiber provided by the application has the advantages of low cost, high production efficiency, high yield and no adhesion problem.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is a schematic view of a carbonization apparatus used in an embodiment of the present application;
FIG. 2 is a partial process flow diagram of an embodiment of the present application;
FIG. 3 is a graph comparing pore size distribution intervals of activated carbon fibers obtained in example 5 of the present application and commercially available products;
FIG. 4 is a graph comparing the volatile contents of the activated carbon fiber obtained in example 5 of the present application with those of a commercially available product.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
Soaking the viscose fiber felt in a 5% phosphoric acid solution at 65 ℃ for 10min, wherein the mass ratio of phosphoric acid in the phosphoric acid aqueous solution to viscose fiber is 0.2: phosphoric acid: water = 1. Then carbonizing by using carbonizing equipment shown in figure 1, wherein the carbonizing process selects gradient temperature rise: the temperature of the first gradient is 70 ℃ and the time is 18min; the temperature of the second gradient is 96 ℃, and the time is 20min; the temperature of the third gradient is 140 ℃ and the time is 30min; the fourth gradient time is 0; the temperature of the fifth gradient is 280 ℃ and the time is 8min; the temperature of the sixth gradient is 450 ℃ and the time is 90min. As shown in fig. 2, after carbonization, the product is cooled to room temperature, and then washed by 3 stages of countercurrent water, wherein the temperature of water washing is 75 ℃, the mass of water used for water washing is 12 times of the mass of the activated carbon fiber, and the retention time of each stage of water washing is 15min. Then, blast drying is carried out, the drying temperature is 90 ℃, and the hot air circulation amount is 900m 3 and/kgACF to obtain the activated carbon fiber.
The measurement results are: yield of Activated Carbon Fiber (ACF) is 44%, ash content is 1.3%, and ACF specific surface is 1374m 2 The total pore volume is 0.4750cc/g, the pore volume of 1-2nm accounts for 30.52% of the total pore volume, the problem of doubling is not generated, the fiber felt is soft, and the fiber felt is 200mg/m 3 The xylene dynamic adsorption capacity of (a) is 25%.
Example 2
Soaking the solvent-process cellulose fiber paper in a phosphoric acid solution with the concentration of 8% at 45 ℃ for 540min, wherein the mass ratio of phosphoric acid in the phosphoric acid aqueous solution to the solvent-process cellulose fiber is 0.3: phosphoric acid: water = 1. Then carbonizing, wherein the carbonization process selects gradient temperature rise: the temperature of the first gradient is 80 ℃ and the time is 10min; the temperature of the second gradient is 96 ℃ and the time is 15min; the temperature of the third gradient is 160 ℃ and the time is 15min; the temperature of the fourth gradient is 200 ℃ and the time is 20min; the temperature of the fifth gradient is 300 ℃ and the time is 20min; the temperature of the sixth gradient is 400 ℃ and the time is 30min. Cooling to room temperature after carbonization, then adopting 4-stage countercurrent washing, wherein the washing temperature is 95 ℃, and the mass of water used for washing is equal to that of the activated carbon fiber1 time, and the retention time of each stage of water washing is 5min. Then, air-blast drying is carried out, the drying temperature is 120 ℃, and the hot air circulation amount is 300m 3 and/kgACF to obtain the activated carbon fiber.
The measurement results are: yield of Activated Carbon Fiber (ACF) is 43%, ash content is 0.93%, and specific surface area of ACF is 1892m 2 The total pore volume is 0.6483cc/g, the pore volume of 1-2nm accounts for 60.14 percent of the total pore volume, the problem of doubling is not caused, the fiber felt is soft, and the fiber felt is 200mg/m 3 The xylene dynamic adsorption capacity of (a) was 36%.
Example 3
Soaking the copper ammonia fiber felt in a 10% phosphoric acid solution at 30 ℃ for 30min, wherein the mass ratio of phosphoric acid in the phosphoric acid solution to the copper ammonia fiber is 0.5: phosphoric acid: water = 1. Then carbonizing, wherein the carbonization process selects gradient temperature rise: the temperature of the first gradient is 60 ℃ and the time is 15min; the temperature of the second gradient is 110 ℃ and the time is 20min; the temperature of the third gradient is 150 ℃ and the time is 40min; the temperature of the fourth gradient is 250 ℃ and the time is 10min; the time of the fifth gradient is 0; the temperature of the sixth gradient is 400 ℃ and the time is 60min. And cooling to room temperature after the carbonization is finished, and then adopting 5-grade countercurrent water washing, wherein the temperature of the water washing is 80 ℃, the mass of water used in the water washing is 6 times of that of the activated carbon fiber, and the retention time of each grade of water washing is 20min. Then, forced air drying is carried out, the drying temperature is 100 ℃, and the hot air circulation amount is 600m 3 and/kgACF to obtain the activated carbon fiber.
The measurement results are: yield of Activated Carbon Fiber (ACF) is 43%, ash content is 1.28%, and ACF specific surface is 1963m 2 The total pore volume is 0.6954cc/g, the pore volume of 1-2nm accounts for 63.29% of the total pore volume, no doubling problem exists, the fiber felt is soft, and the fiber felt is 200mg/m 3 The xylene dynamic adsorption capacity of (a) was 39%.
Example 4
Soaking the viscose fiber cloth in 5% phosphoric acid solution at 25 ℃ for 200min, wherein the mass ratio of phosphoric acid in the phosphoric acid solution to the viscose fiber cloth is 0.4: phosphoric acid: water = 1. Then carbonizing, wherein the carbonization process selects gradient temperature rise: first gradientThe temperature is 60 ℃ and the time is 20min; the temperature of the second gradient is 90 ℃ and the time is 30min; the temperature of the third gradient is 150 ℃ and the time is 15min; the temperature of the fourth gradient is 250 ℃ and the time is 15min; the time of the fifth gradient is 0; the sixth gradient temperature is 350 deg.C and time is 60min. And cooling to room temperature after the carbonization is finished, and then adopting 3-stage countercurrent water washing, wherein the water washing temperature is 90 ℃, the mass of water used for water washing is 10 times of that of the activated carbon fiber, and the retention time of each stage of water washing is 15min. Then, drying by blowing at 110 deg.C with hot air circulation amount of 800m 3 and/kgACF to obtain the activated carbon fiber.
The measurement results are: yield of Activated Carbon Fiber (ACF) is 44%, ash content is 0.86%, and specific surface area of ACF is 1298m 2 The total pore volume is 0.4472cc/g, the pore volume of 1-2nm accounts for 28.47% of the total pore volume, no doubling problem exists, the fiber felt is soft, and the fiber felt is 200mg/m 3 The xylene dynamic adsorption capacity of (2) was 20%.
Example 5
Soaking the solvent-process cellulose fiber felt in a 13% phosphoric acid solution at 20 ℃ for 600min, wherein the mass ratio of phosphoric acid in the phosphoric acid aqueous solution to the solvent-process cellulose fiber felt is 0.5: phosphoric acid: water = 1. Then carbonizing, wherein the carbonization process selects gradient temperature rise: the temperature of the first gradient is 50 ℃ and the time is 30min; the temperature of the second gradient is 90 ℃ and the time is 32min; the temperature of the third gradient is 120 ℃ and the time is 15min; the temperature of the fourth gradient is 250 ℃ and the time is 20min; the time of the fifth gradient is 0; the temperature of the sixth gradient is 300 deg.C and the time is 90min. Cooling to room temperature after carbonization, and then adopting 3-stage countercurrent washing, wherein the washing temperature is 70 ℃, the mass of water used for washing is 3 times of that of the activated carbon fiber, and the retention time of each stage of washing is 10min. Then, forced air drying is carried out, the drying temperature is 100 ℃, and the hot air circulation amount is 400m 3 and/kgACF to obtain the activated carbon fiber.
The measurement results are: yield of Activated Carbon Fiber (ACF) is 42%, ash content is 1.09%, and ACF specific surface is 2059m 2 (ii)/g, the total pore volume is 0.7162cc/g, the pore volume of 1-2nm accounts for 72.51% of the total pore volume,has no doubling problem, the fiber felt is soft and 200mg/m 3 The xylene dynamic adsorption capacity of (a) was 41%.
Example 6
Soaking the fibrilia cloth in 7% phosphoric acid solution at 35 ℃ for 300min, wherein the mass ratio of phosphoric acid in the phosphoric acid solution to the fibrilia cloth is 0.8: phosphoric acid: water = 1. Then carbonizing, wherein the carbonization process selects gradient temperature rise: the temperature of the first gradient is 65 ℃ and the time is 25min; the temperature of the second gradient is 110 ℃ and the time is 20min; the temperature of the third gradient is 150 ℃ and the time is 35min; the temperature of the fourth gradient is 230 ℃ and the time is 15min; the temperature of the fifth gradient is 280 ℃, and the time is 10min; the temperature of the sixth gradient is 450 ℃ and the time is 60min. And cooling to room temperature after the carbonization is finished, and then adopting 4-stage countercurrent water washing, wherein the water washing temperature is 85 ℃, the mass of water used for water washing is 8 times of that of the activated carbon fiber, and the retention time of each stage of water washing is 15min. Then, air-blast drying is carried out, the drying temperature is 110 ℃, and the hot air circulation amount is 600m 3 and/kgACF to obtain the activated carbon fiber.
The measurement results are: yield of Activated Carbon Fiber (ACF) is 40%, ash content is 1.29%, and specific surface area of ACF is 1536m 2 The total pore volume is 0.5628cc/g, the pore volume of 1-2nm accounts for 49.28% of the total pore volume, the problem of doubling is not generated, the fiber felt is soft, and the fiber felt is 200mg/m 3 The xylene dynamic adsorption capacity of (a) was 31%.
Therefore, the preparation method of the activated carbon fiber provided by the application avoids the problem of filament adhesion of the activated carbon fiber in the carbonization process, improves the yield of the activated carbon fiber, increases the strength of the activated carbon fiber, reduces the ash content, improves the specific surface of the activated carbon fiber, and prepares the activated carbon fiber which is softer and has better performance.
Comparative example 1
Soaking the viscose fiber cloth in 20% phosphoric acid solution for 16 hours at room temperature, wherein the mass ratio of the phosphoric acid aqueous solution to the viscose fiber is 1.
The measurement results are: yield of Active Carbon Fiber (ACF) is 38%, ACF specific surface is 702m 2 (g), ash content is 1.5%, and the fiber felt is soft and poor in strength.
Comparative example 2
Dipping viscose fiber filaments in 35% phosphoric acid solution for 12 hours at room temperature, wherein the mass ratio of phosphoric acid aqueous solution to viscose fiber is 1.
The measurement results are: the yield of the Activated Carbon Fiber (ACF) is 40 percent, and the specific surface area of the ACF is 1117m 2 (g), ash content is 1.8%, and the fiber felt is soft and has poor strength.
Comparative example 3
A solvent process cellulose fiber sample a (washingegeli-a 900) and a viscose fiber sample B (washingegeli-B1200) on the current market were collected and compared with the activated carbon fiber sample prepared in example 5 to determine the differences in specific surface area and pore size distribution, and the results are shown in table 1 below, the pore size distribution interval is shown in fig. 3, and the volatile content ratio is shown in fig. 4.
TABLE 1 comparison of Performance parameters
As can be seen from the above Table 1, the specific surface area, the total pore volume, the volatile content and the xylene dynamic adsorption capacity of the activated carbon fiber obtained by the method are better than those of the commercially available product, and the pore size distribution is more reasonable.
To further illustrate the composition of the activated carbon fibers prepared herein and to compare with commercially available products, samples of activated carbon fibers currently on the market were collected and compared with the sample prepared in example 4 to determine the difference in elemental composition. The results are shown in table 2 below:
TABLE 2 element content
As can be seen from table 2, the activated carbon fibers obtained in the present application have an oxygen content higher than that of commercially available products and a nitrogen content lower than that of commercially available products.
The preparation method of the activated carbon fiber provided by the application has the advantages of low cost, high production efficiency, high yield and no adhesion problem; the application provides an activated carbon fiber, specific surface area is big, the ash content is low, intensity is high, adsorbs and desorption properties is good.
Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present application shall be included in the protection scope of the present application. While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (5)
1. A method for preparing activated carbon fibers is characterized by comprising the following steps:
using phosphoric acid aqueous solution with the mass fraction of 5-13% to dip raw material artificial fiber and/or natural fiber, carbonizing after drying, cooling, washing and drying to obtain the activated carbon fiber, wherein the ash content of the activated carbon fiber is 0.8-3 wt%, and the specific surface area is 1000m 2 /g-2200m 2 The total pore volume is 0.4120cc/g-0.8370cc/g, the 1-2nm pore volume ratio is 28% -75%,200mg/m 3 The xylene adsorption capacity is 20-45%;
the dipping temperature is 10-65 ℃; the drying mode before carbonization is air drying or hot air blow drying at 20-50 ℃, and after drying is finished, the mass ratio of the artificial fiber or natural fiber to the phosphoric acid to the water is 1: (0.2-0.8): (0-1); the carbonization is carried out in the air atmosphere or inert gas atmosphere by adopting a gradient temperature rise method, wherein the temperature of a first gradient is 50-80 ℃, and the time is 10-30min; the temperature of the second gradient is 90-110 ℃, and the time is 15-32min; the temperature of the third gradient is 120-160 ℃, and the time is 15-40min; the temperature of the fourth gradient is 200-250 ℃ and the time is 10-20min; the temperature of the fifth gradient is 280-300 ℃, and the time is 0-20min; the temperature of the sixth gradient is 300-450 ℃, and the time is 10-90min; the water washing adopts a multi-stage countercurrent water washing mode, the water washing temperature is 65-95 ℃, and the mass of water used for water washing is 1-12 times of the mass of the activated carbon fiber; the stage number is 3-5, and the retention time of each stage of water washing is 5-20min.
2. The preparation method according to claim 1, characterized in that the raw material is paper, felt or cloth processed by respective raw materials of artificial fiber and/or natural fiber, wherein the artificial fiber comprises one or more of viscose fiber, solvent-process cellulose fiber and cuprammonium fiber; the natural fiber comprises one or more of hemp fiber, cotton fiber and silk fiber.
3. The method for preparing the nano-particles according to claim 1, wherein the dipping time is 10-600min, and the dipping temperature is 40-65 ℃; after the impregnation is finished, the mass ratio of the artificial fiber or the natural fiber as the raw material to the phosphoric acid to the water is 1: (0.2-0.8): (1.8-9.2).
4. The method of claim 1, wherein the end point of the cooling is room temperature.
5. The method according to any one of claims 1 to 4, wherein the temperature of drying after carbonization is 90 to 120 ℃; the drying is carried out by blowing, and the hot air circulation amount is 300-900m 3 The activated carbon fiber is/kg.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910906928.9A CN112619599B (en) | 2019-09-24 | 2019-09-24 | Active carbon fiber and preparation method thereof |
| PCT/CN2020/105817 WO2021057247A1 (en) | 2019-09-24 | 2020-07-30 | Activated carbon fiber and preparation method therefor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910906928.9A CN112619599B (en) | 2019-09-24 | 2019-09-24 | Active carbon fiber and preparation method thereof |
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| CN1295142A (en) * | 2000-10-28 | 2001-05-16 | 中山大学 | Phosphoric acid activation process of producing active carbon fiber |
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| CN109487372A (en) * | 2017-09-11 | 2019-03-19 | 刘小蕾 | A kind of preparation method of plant Carbon fibe |
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| EP1622830A2 (en) * | 2003-05-09 | 2006-02-08 | McGill University | Process for the production of activated carbon |
| US7727932B2 (en) * | 2005-12-16 | 2010-06-01 | Ut-Battelle, Llc | Activated carbon fibers and engineered forms from renewable resources |
| CN100564623C (en) * | 2007-04-29 | 2009-12-02 | 武汉理工大学 | A kind of preparation method of vegetable active charcoal fibre columns |
| CN102140709B (en) * | 2011-01-27 | 2012-11-07 | 济南大学 | Microporous activated carbon fiber and preparation method thereof |
| CN104016343B (en) * | 2013-02-28 | 2016-12-07 | 中国科学院理化技术研究所 | A kind of preparation method of the bamboo fiber-based NACF of high specific surface micro-pore |
| CN103225133A (en) * | 2013-02-28 | 2013-07-31 | 江苏竹溪活性炭有限公司 | Active carbon fiber and preparation method thereof |
| CN106276897A (en) * | 2016-08-11 | 2017-01-04 | 潘忠宁 | A kind of preparation method of phosphoric acid activation monkey grass |
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| US5102855A (en) * | 1990-07-20 | 1992-04-07 | Ucar Carbon Technology Corporation | Process for producing high surface area activated carbon |
| CN1114633A (en) * | 1994-07-03 | 1996-01-10 | 中国科学院长春应用化学研究所 | Method for preparation of viscose fibre active carbon |
| CN1295142A (en) * | 2000-10-28 | 2001-05-16 | 中山大学 | Phosphoric acid activation process of producing active carbon fiber |
| CN109487372A (en) * | 2017-09-11 | 2019-03-19 | 刘小蕾 | A kind of preparation method of plant Carbon fibe |
| CN108970578A (en) * | 2018-07-19 | 2018-12-11 | 深圳市环球绿地新材料有限公司 | The preparation and regeneration method of spherical activated charcoal |
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