CN112076720B - Activated carbon fiber and preparation method thereof - Google Patents
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- 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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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28014—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 form
- B01J20/28023—Fibres or filaments
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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 relates to the field of activated carbon fibers, and particularly provides an activated carbon fiber and a preparation method thereof. The activated carbon fiber has no adhesion and hardening, and the specific surface area of the activated carbon fiber is 1800m2/g‑2500m2Per g, total pore volume of 0.57cm3/g‑0.93cm3The ratio of pores below 0.8nm is 37-60%, the ratio of pores between 0.8 and 2nm is 37-60%, the ratio of pores above 2nm is less than 3%, and the yield is more than 40%. The activated carbon fiber provided by the application has high phosphoric acid loading rate, large specific surface area, tensile breaking strength of 7-12MPa, no adhesion, hardening and easy pulverization problems, and has excellent adsorption and desorption properties; the preparation method has the advantages of high product yield, strong hydrophobicity and excellent performance.
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
At present, the preparation of activated carbon fiber from domestic artificial fiber is mainly a physical activation method, the preparation process comprises the steps of impregnating felt or cloth of artificial fiber (including organic fibers such as viscose fiber, solvent method cellulose fiber, copper ammonia fiber and the like) with phosphate solution with certain concentration, drying, and then carbonizing and activating, wherein common activating agents are water vapor and carbon dioxide.
The process method has the following problems:
(1) the physical activation method has the advantages that the water-carbon reaction is violent in the activation stage of the preparation process, so that the yield of the activated carbon fiber product is low, and the yield is continuously reduced along with the increase of the specific surface area, wherein the specific surface area is usually less than 1200m2The yield of the activated carbon fiber carbon is less than 23 percent per gram, and the specific surface area is more than 1500m2The yield of the activated carbon fiber carbon is less than 16 percent per gram, and the specific surface area isThe higher the yield, the lower the production cost.
(2) The specific surface of the product is generally not more than 1800m2And/g, otherwise, the strength of the activated carbon fiber is deteriorated after deep activation, so that the pulverization problem is caused, and the use of the product is influenced.
The chemical activation method of phosphoric acid can solve the above problems well, and the specific surface area of the chemical activated carbon fiber of phosphoric acid can be increased to the level of super activated carbon (2500 m)2Per gram), the product yield is 40-45%, and the yield does not decrease with the increase of the specific surface. However, the method has the following problems:
the specific surface area of the activated carbon fiber by the phosphoric acid chemical activation method is directly influenced by the load rate, the phosphoric acid load rate is too low, the pyrolysis temperature of the product is high, the carbonization is not thorough, and the prepared activated carbon fiber has smaller specific surface area (less than 1000 m)2(g), the product performance is poor, and the market value is not high; the phosphoric acid loading rate is too high (the ratio of the artificial fiber to the phosphoric acid is more than 1:0.5), the dissolution and hydrolysis of the artificial fiber are enhanced by the phosphoric acid, the artificial fiber is pulverized in the drying process, or the activated carbon fiber is bonded and hardened in the carbonization stage, and in order to avoid the problem of fiber hardening, the phosphoric acid loading rate of the ACF by the existing phosphoric acid chemical method is usually lower than 60%, so that the specific surface area of the existing product is smaller, and the market popularization value is not high.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide the activated carbon fiber which has high phosphoric acid loading rate, large specific surface area, high strength, no adhesion, hardening and easy pulverization problems and has excellent adsorption and desorption performances.
The second purpose of the invention is to provide a preparation method of activated carbon fiber, which has high product yield and excellent performance.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
an activated carbon fiber which is not sticky and hardened, has an ash content of 1.2-2.5 wt% and a specific surface area of 1800m2/g-2500m2Per g, total pore volume of 0.57cm3/g-0.93cm3/g，0The ratio of pores below 8nm is 37-60%, the ratio of pores between 0.8-2nm is 37-60%, and the ratio of pores above 2nm is less than 3%.
The xylene saturated adsorption capacity (calculated by weight) of the activated carbon fiber is 35-60%.
The preparation method of the activated carbon fiber comprises the steps of dipping the activated carbon fiber by using a phosphoric acid aqueous solution for one time, drying the dipped activated carbon fiber for one time and then carbonizing the dipped activated carbon fiber for one time; then secondary phosphoric acid dipping, secondary drying, secondary carbonization, water washing and drying are carried out to obtain the activated carbon fiber; the raw materials are artificial fibers and/or natural fibers.
The raw materials are paper, felt or cloth processed by artificial fibers and/or natural fibers, and the artificial fibers comprise one or more of viscose fibers, solvent-process cellulose fibers and cuprammonium fibers; the natural fiber comprises one or more of hemp fiber, cotton fiber and silk fiber.
After the primary impregnation, the mass concentration of the phosphoric acid aqueous solution is 5-30%; the temperature of the primary drying is 20-120 ℃, and the time is 1-12 h; and after the primary drying is finished, the mass ratio of the artificial fiber or the natural fiber to the pure phosphoric acid is 1: 0.2-0.5. At a lower drying temperature, the drying time can be prolonged, and the peripheral hardening phenomenon of the fiber caused by uneven phosphoric acid loading is favorably improved.
The primary carbonization is carried out in an inert gas atmosphere by adopting a gradient temperature raising method:
the temperature of the first gradient is 50-100 ℃ and the time is 5-30 min; the temperature of the second gradient is 100-150 ℃, and the time is 8-30 min; the temperature of the third gradient is 150-; the temperature of the fourth gradient is 200-300 ℃, and the time is 0-30 min.
The flow rate of the inert gas is controlled to be 5-20L/min.
Controlling the primary loading rate of the phosphoric acid to be 20-50 percent, namely the mass ratio of the artificial fiber or the natural fiber to the phosphoric acid is 1: 0.2-0.5; the primary carbonization temperature is 150-300 ℃. Phosphoric acid load rate can direct influence the pyrolysis temperature of flooding felt, and along with the increase of load rate, the pyrolysis temperature of flooding felt can reduce, and after the load rate exceeded a definite value, the pyrolysis temperature region can reach stably. The primary carbonization temperature can directly influence the performance of the product, the primary carbonization temperature is too low, more cellulose characteristics are kept in the carbonized original felt, the adhesion problem is easy to occur in the secondary carbonization process, the adhesion and hardening problem in the secondary carbonization process can be solved even if the primary carbonization temperature is too high, the permeation of phosphoric acid in the secondary impregnation process is not facilitated, and the final performance of the activated carbon fiber can be influenced.
When the secondary phosphoric acid is used for dipping, the concentration of the phosphoric acid aqueous solution is 10-30%, and the mass ratio of the fiber after secondary loading to the pure phosphoric acid is 1: 0.5-0.9.
By reducing the phosphoric acid loading rate in the primary impregnation process, the problems of product adhesion and hardening, poor flexibility and strength and the like caused by the dissolution and hydrolysis of excessive phosphoric acid under high phosphoric acid loading rate are solved; through the secondary loading process, the total phosphoric acid loading rate is improved, and the problems of small specific surface area of products, poor adsorption performance of VOCs and the like when the phosphoric acid loading rate is too low are solved.
The temperature of the secondary drying is 80-150 ℃, and the time is 1-3 h; and after the secondary drying is finished, the mass ratio of the fiber to the pure phosphoric acid is 1: 0.5-0.9.
And the secondary carbonization is carried out by adopting a gradient temperature raising method under the atmosphere of inert gas:
the temperature of the first gradient is 100-200 ℃, and the time is 10-30 min; the temperature of the second gradient is 200-300 ℃, and the time is 5-30 min; the temperature of the third gradient is 300-400 ℃, and the time is 5-40 min; the temperature of the fourth gradient is 400-900 ℃, and the time is 0-30 min.
The flow rate of the inert gas is controlled to be 5-20L/min.
The yield of the activated carbon fiber is more than 40 percent.
Compared with the prior art, the invention has the beneficial effects that:
(1) compared with a physical activation process, the secondary load phosphoric acid chemical activation process can improve the specific surface area of the activated carbon fiber to 1800m2/g-2500m2The yield is up to more than 40 percent, the cost is reduced, and the size shrinkage rate is reduced.
(2) Compared with the existing chemical activation process, the method overcomes the defects of small specific surface area and poor performance of the product under low phosphoric acid loading rate, and the defects of brittle fiber, poor strength and easy pulverization under high phosphoric acid loading rate, and has excellent adsorption and desorption performances.
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 process flow diagram used in an embodiment of the present application.
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
An activated carbon fiber which is not sticky and hardened, has an ash content of 1.25 wt% and a specific surface area of 2158m2(g) the fiber felt is soft, and the pore volume is 0.77cm3In terms of the ratio of pores having a diameter of 0.8nm or less, about 60%, from 0.8 to 2nm, about 37%, and more than 2nm, about 3%.
The preparation method is as shown in the process flow shown in figure 1, and specifically comprises the following steps: and (3) mixing and impregnating the copper ammonia fiber felt with 15% phosphoric acid solution, wherein the mass ratio of the fiber to the phosphoric acid after primary impregnation and loading is 1: 0.35, i.e., the primary loading of phosphoric acid was 35%. Drying with 50 deg.C hot air for 5 hr, carbonizing in nitrogen atmosphere, and performing gradient heating process, wherein the first gradient temperature is 90 deg.C for 10min, the second gradient temperature is 120 deg.C for 30min, and the third gradient temperature is 180 deg.C for 20 min; carrying out secondary phosphoric acid loading on the product obtained by primary carbonization, wherein the mass ratio of the fiber to the total phosphoric acid after the secondary loading is 1:0.8, and the total loading rate of the phosphoric acid reaches 80%; and then carrying out secondary drying at the temperature of 100 ℃ for 2h, carrying out secondary carbonization on the dried product, wherein the secondary carbonization is still a gradient temperature rise process, namely the temperature of the first gradient is 100 ℃ for 10min, the temperature of the second gradient is 200 ℃ for 20min, and the temperature of the third gradient is 350 ℃ for 10 min. Finally, washing with water and drying for three times to obtain the product. The phosphoric acid after washing can be recycled.
Finally, the tensile breaking strength of the activated carbon fiber is 11.5MPa, the activated carbon fiber is not hardened, the yield is 45 percent, and the saturated adsorption capacity (calculated by weight) of the dimethylbenzene is 45.97 percent.
Example 2
An activated carbon fiber which is not sticky and hardened, has an ash content of 2.3 wt% and a specific surface area of 2229m2G, the fiber felt is soft, and the pore volume is 0.93cm3In terms of the ratio of pores having a diameter of 0.8nm or less, about 37% in terms of the ratio of pores having a diameter of 0.8 to 2nm, about 60% in terms of the ratio of pores having a diameter of 2nm or more, and about 3% in terms of the ratio of pores having a diameter of 2nm or more.
The preparation method comprises the following steps: the solvent method cellulose fiber paper is mixed and soaked with 20% phosphoric acid solution, the mass ratio of the fiber to the phosphoric acid after one-time soaking and loading is 1:0.4, namely the one-time loading rate of the phosphoric acid is 40%. Drying at 70 deg.C for 2 hr, carbonizing in nitrogen atmosphere, and heating in gradient manner at first gradient temperature of 100 deg.C for 10min, second gradient temperature of 150 deg.C for 10min, and third gradient temperature of 200 deg.C for 20 min; carrying out secondary phosphoric acid loading on the product obtained by primary carbonization, wherein the phosphoric acid concentration in the secondary loading process is 25%, the mass ratio of the fiber to the total phosphoric acid after the secondary loading is 1:0.85, and the total phosphoric acid loading rate reaches 85%; and then carrying out secondary drying at the drying temperature of 100 ℃ for 2h, carrying out secondary carbonization on the dried product, wherein the secondary carbonization is still a gradient temperature rise process, namely the temperature of the first gradient is 150 ℃ for 15min, the temperature of the second gradient is 250 ℃ for 15min, and the temperature of the third gradient is 350 ℃ for 20 min. Finally, washing with water and drying for three times to obtain the product. The phosphoric acid after washing can be recycled.
The final tensile breaking strength of the activated carbon fiber is 10.2MPa, no hardening occurs, the yield is 43 percent, and the saturated adsorption capacity (calculated by weight) of the dimethylbenzene is 53.02 percent.
Example 3
An activated carbon fiber which is not sticky and hardened, has an ash content of 1.84 wt% and a specific surface area of 2299m2(g) the fiber felt is soft, and the pore volume is 0.92cm3In terms of the ratio of pores having a size of 0.8nm or less, about 41% by weight, and about 59% by weight, having no pores having a size of 2nm or more, in the range of 0.8 to 2 nm.
The preparation method comprises the following steps: and (3) mixing and impregnating fibrilia and 10% phosphoric acid solution, wherein the mass ratio of the fibrilia to the phosphoric acid after primary impregnation loading is 1: 0.35, i.e., the primary loading of phosphoric acid was 35%. Drying at 80 ℃ for 1.5h, then carrying out primary carbonization treatment in nitrogen atmosphere, wherein the primary carbonization selects a gradient temperature rise process, namely the temperature of a first gradient is 70 ℃ for 5min, the temperature of a second gradient is 130 ℃ for 30min, the temperature of a third gradient is 160 ℃ for 20min, and the temperature of a fourth gradient is 220 ℃ for 5 min; carrying out secondary phosphoric acid loading on the product obtained by primary carbonization, wherein the concentration of phosphoric acid loaded by the secondary phosphoric acid is 30 percent, the mass ratio of the fiber to the total phosphoric acid after the secondary loading is 1:0.85, and the total loading rate of the phosphoric acid reaches 85 percent; and then carrying out secondary drying at the drying temperature of 90 ℃ for 1.5h, carrying out secondary carbonization on the dried product, wherein the secondary carbonization is still a gradient temperature rise process, namely the temperature of the first gradient is 150 ℃ for 10min, the temperature of the second gradient is 250 ℃ for 20min, the temperature of the third gradient is 350 ℃ for 10min, and the temperature of the fourth gradient is 400 ℃ for 10 min. And finally, washing and drying to obtain the product. The phosphoric acid after washing can be recycled.
The final tensile breaking strength of the activated carbon fiber is 11.6MPa, no hardening occurs, the yield is 42 percent, and the saturated adsorption capacity (calculated by weight) of the dimethylbenzene is 58.44 percent.
Example 4
An activated carbon fiber which is not sticky and hardened, has an ash content of 2.15 wt% and a specific surface area of 2302m2G, the fiber felt is soft, and the pore volume is 0.93cm3(ii)/g, the ratio of pores having a size of 0.8nm or less is about 47%, and the ratio of pores having a size of 0.8 to 2nm is about 53%No pores larger than 2 nm.
The preparation method comprises the following steps: and (3) mixing and impregnating the copper ammonia fiber felt with 25% phosphoric acid solution, wherein the mass ratio of the fiber to the phosphoric acid after primary impregnation and loading is 1: 0.35, i.e., the primary loading of phosphoric acid was 35%. Drying at 65 ℃ for 3h, then carrying out primary carbonization treatment in a nitrogen atmosphere, wherein the primary carbonization selects a gradient temperature rise process, namely the temperature of a first gradient is 80 ℃ for 9min, the temperature of a second gradient is 110 ℃ for 15min, the temperature of a third gradient is 150 ℃ for 20min, and the temperature of a fourth gradient is 200 ℃ for 20 min; carrying out secondary phosphoric acid loading on the product obtained by primary carbonization, wherein the concentration of phosphoric acid loaded by the secondary phosphoric acid is 26 percent, the mass ratio of the fiber to the total phosphoric acid after the secondary loading is 1:0.75, and the total loading rate of the phosphoric acid reaches 75 percent; and then carrying out secondary drying at the drying temperature of 120 ℃ for 1h, carrying out secondary carbonization on the dried product, wherein the secondary carbonization is still a gradient temperature rise process, namely the temperature of the first gradient is 150 ℃ for 15min, the temperature of the second gradient is 250 ℃ for 20min, the temperature of the third gradient is 350 ℃ for 5min, and the temperature of the fourth gradient is 450 ℃ for 15 min. And finally, washing and drying to obtain the product. The phosphoric acid after washing can be recycled.
Finally, the tensile breaking strength of the activated carbon fiber is 7.6MPa, the activated carbon fiber is not hardened and is a hydrophobic material, the yield is 41 percent, and the saturated adsorption capacity (calculated by weight) of the dimethylbenzene is 53.39 percent.
Example 5
An activated carbon fiber which is non-sticky and hardened, has an ash content of 2.08 wt% and a specific surface area of 2087m2(g) the fiber felt is soft, and the pore volume is 0.82cm3In terms of the ratio of pores having a size of 0.8nm or less, the ratio of pores having a size of 0.8 to 2nm is about 45%, the ratio of pores having a size of about 55%, and no pores having a size of 2nm or more.
The preparation method comprises the following steps: the solvent method cellulose fiber felt is mixed and soaked with 22% phosphoric acid solution, so that the mass ratio of the fiber to the phosphoric acid after primary soaking and loading is 1:0.5, namely the primary loading rate of the phosphoric acid is 50%. Drying at 70 deg.C for 2 hr, carbonizing in nitrogen atmosphere, and selectively heating in gradient manner at first gradient temperature of 100 deg.C for 15min, second gradient temperature of 150 deg.C for 15min, and third gradient temperature of 200 deg.C for 15 min; carrying out secondary phosphoric acid loading on the product obtained by primary carbonization, wherein the concentration of phosphoric acid loaded by the secondary phosphoric acid is 25 percent, the mass ratio of the fiber to the total phosphoric acid after the secondary loading is 1:0.9, and the total phosphoric acid loading rate reaches 90 percent; and then carrying out secondary drying at the temperature of 100 ℃ for 2h, carrying out secondary carbonization on the dried product, wherein the secondary carbonization is still a gradient temperature rise process, namely the temperature of the first gradient is 150 ℃ for 10min, the temperature of the second gradient is 250 ℃ for 10min, the temperature of the third gradient is 400 ℃ for 10min, and the temperature of the fourth gradient is 550 ℃ for 10 min. And finally, washing and drying to obtain the product. The phosphoric acid after washing can be recycled.
Finally, the tensile breaking strength of the activated carbon fiber is 8.4MPa, the activated carbon fiber is not hardened, the activated carbon fiber is a hydrophobic material, the yield is 40%, and the saturated adsorption capacity (calculated by weight) of the dimethylbenzene is 48.75%.
Comparative example 1
Mixing a solvent method cellulose fiber felt with 10% phosphoric acid solution, soaking for 60min at 50 ℃, wherein the mass ratio of the soaked and loaded fiber to the phosphoric acid is 1:0.5, namely the loading rate of the phosphoric acid is 50%, drying for 2h at 70 ℃, and then carrying out carbonization treatment, wherein the carbonization process selects a gradient heating method, the temperature of a first gradient is 100 ℃, and the time is 20 min; the temperature of the second gradient is 250 ℃ and the time is 20 min; the temperature of the third gradient is 450 ℃ and the time is 60 min; and cooling to room temperature after carbonization, washing with water to remove residual phosphoric acid, and drying at 110 ℃ to obtain the activated carbon fiber. The yield is 33 percent, the ash content is 1.75 percent, and the specific surface area is 1034m2The fiber felt is soft, the tensile breaking strength is 5.4MPa, the pores with the diameter less than 0.8nm account for 51 percent, the pores with the diameter of 0.8-2nm account for 47 percent, the pores with the diameter more than 2nm account for 2 percent, and the saturated adsorption capacity (calculated by weight) of the dimethylbenzene is 21.83 percent.
Comparative example 2
A viscose fiber sample A (Huashijie-B1200) on the current market is collected, and the product performance is tested, so that the ash content of the product is 1.75 percent, and the specific surface area is 1500m2G, the fiber felt is soft, and the tensile breaking strength is 3.1MPa65% of pores with the diameter less than 0.8nm, 35% of pores with the diameter of 0.8-2nm, no pores with the diameter of more than 2nm, and the saturated adsorption capacity (calculated by weight) of dimethylbenzene is 35%.
It can be seen from the above examples and comparative examples that after secondary loading and secondary carbonization, the yield and specific surface area of the activated carbon fiber are significantly increased, there is no problem of adhesion and hardening and easy pulverization, and it has excellent adsorption and desorption properties.
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 (7)
1. The activated carbon fiber is characterized by being non-sticky and hardened, having tensile breaking strength of 7-12MPa and specific surface area of 1800m 2 /g-2500m 2Per g, total pore volume of 0.57cm3 /g-0.93cm 3 The proportion of pores below 0.8nm is 37-60%, the proportion of pores between 0.8-2nm is 37-60%, and the proportion of pores above 2nm is less than 3%;
the preparation method of the activated carbon fiber comprises the steps of carrying out primary impregnation on raw materials by using a phosphoric acid aqueous solution, carrying out primary carbonization after primary drying, and then carrying out secondary phosphoric acid impregnation, secondary drying, secondary carbonization, washing and drying to obtain the activated carbon fiber, wherein the raw materials are artificial fibers and/or natural fibers;
after the primary drying is finished, the mass ratio of the artificial fiber or the natural fiber to the pure phosphoric acid is 1: 0.2-0.5;
the primary carbonization is carried out in an inert gas atmosphere by adopting a gradient temperature raising method:
the temperature of the first gradient is 50-100 ℃ and the time is 5-30 min; the temperature of the second gradient is 100-150 ℃, and the time is 8-30 min; the temperature of the third gradient is 150-; the temperature of the fourth gradient is 200-300 ℃, and the time is 0-30 min;
the mass ratio of the fiber to the pure phosphoric acid after the secondary impregnation is 1: 0.5-0.9;
the secondary carbonization is carried out in an inert gas atmosphere by adopting a gradient temperature raising method:
the temperature of the first gradient is 100-; the temperature of the second gradient is 200-300 ℃, and the time is 5-30 min; the temperature of the third gradient is 300-400 ℃, and the time is 5-40 min; the temperature of the fourth gradient is 400-900 ℃, and the time is 0-30 min.
2. The activated carbon fiber of claim 1, wherein the activated carbon fiber has a xylene saturation adsorption capacity of 35% to 60% by weight.
3. The activated carbon fiber according to claim 1, wherein the raw material is paper, felt or cloth processed from artificial fiber and/or natural fiber, 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.
4. The activated carbon fiber according to claim 1, wherein the concentration of the phosphoric acid solution in the primary impregnation process is 5-30%; the primary drying temperature is 20-120 ℃, and the time is 1-12 h.
5. The activated carbon fiber according to claim 1, wherein the concentration of the phosphoric acid aqueous solution is 10% to 30% at the time of the secondary phosphoric acid impregnation.
6. The activated carbon fiber according to claim 1, wherein the temperature of the secondary drying is 80-150 ℃ and the time is 1-3 h.
7. The activated carbon fiber of claim 1, wherein the activated carbon fiber is activated by heatThe yield of the carbon fiber is more than 40 percent, and the specific surface area is more than 1800m2 /g。
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| WO2004099073A2 (en) * | 2003-05-09 | 2004-11-18 | Mcgill University | Process for the production of activated carbon |
| CN102140709A (en) * | 2011-01-27 | 2011-08-03 | 济南大学 | Microporous activated carbon fiber and preparation method thereof |
| CN103696195A (en) * | 2013-12-11 | 2014-04-02 | 杨学斌 | Secondary carbonization technology for producing activated carbon fibers |
| CN108516548A (en) * | 2018-03-06 | 2018-09-11 | 合肥工业大学 | A kind of preparation method of high mesoporous rate activated carbon and its activated carbon of acquisition |
| CN110172751A (en) * | 2019-05-18 | 2019-08-27 | 孔令孝 | A kind of carbon fibre and its carbonization method |
| CN111172627A (en) * | 2020-01-14 | 2020-05-19 | 安徽工程大学 | Hollow-structure biomass activated carbon fiber and preparation method thereof |
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