CN106702538A - Preparation method of high-performance activated carbon fibers - Google Patents
Preparation method of high-performance activated carbon fibers Download PDFInfo
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 13
- 230000004913 activation Effects 0.000 claims abstract description 56
- 238000000034 method Methods 0.000 claims abstract description 53
- 239000000835 fiber Substances 0.000 claims abstract description 27
- 230000002195 synergetic effect Effects 0.000 claims abstract description 11
- 239000004917 carbon fiber Substances 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 18
- 230000003213 activating effect Effects 0.000 claims description 13
- 230000003647 oxidation Effects 0.000 claims description 13
- 238000007254 oxidation reaction Methods 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 239000011261 inert gas Substances 0.000 claims description 10
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000012190 activator Substances 0.000 claims description 6
- 229910000404 tripotassium phosphate Inorganic materials 0.000 claims description 6
- -1 hydroxyalkyl acrylonitrile Chemical compound 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 4
- 238000002166 wet spinning Methods 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- OWXJKYNZGFSVRC-UHFFFAOYSA-N 1-chloroprop-1-ene Chemical compound CC=CCl OWXJKYNZGFSVRC-UHFFFAOYSA-N 0.000 claims description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 2
- RKAZWPVRTYSEED-UHFFFAOYSA-N 5-methylhex-5-ene-2,4-dione Chemical compound CC(=O)CC(=O)C(C)=C RKAZWPVRTYSEED-UHFFFAOYSA-N 0.000 claims description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 2
- OSDWBNJEKMUWAV-UHFFFAOYSA-N Allyl chloride Chemical compound ClCC=C OSDWBNJEKMUWAV-UHFFFAOYSA-N 0.000 claims description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- 229920000297 Rayon Polymers 0.000 claims description 2
- 230000006690 co-activation Effects 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 238000007334 copolymerization reaction Methods 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 238000000578 dry spinning Methods 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 claims description 2
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000001737 promoting effect Effects 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 238000001994 activation Methods 0.000 abstract description 40
- 238000000746 purification Methods 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract description 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- 238000005311 autocorrelation function Methods 0.000 description 23
- 238000001179 sorption measurement Methods 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 1
Classifications
-
- 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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/16—Chemical after-treatment of artificial filaments or the like during manufacture of carbon by physicochemical methods
-
- 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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/12—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with inorganic substances ; Intercalation
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention relates to a preparation method of high-performance activated carbon fibers, belonging to the technical field of carbon fibers. The method comprises the following steps: on a continuous activation facility, by using polyacrylonitrile-base fibers as the raw material, impregnating a chemical reagent on the surface of the raw material fibers, and preparing the high-performance activated carbon fibers, of which the specific area is not less than 1500m<2>.g<-1> and the tensile strength is not lower than 0.5 GPa, by the aid of a physical-chemical synergic activation process by using the vapor volume percent phi-vapor as the variable (the phi-vapor value is controlled within the range of 0.4-4.5*10<-4>). The method is simple, and has the advantages of high preparation efficiency and lower cost; and the obtained sample has high specific area and excellent mechanical properties, and can form products in various shapes so as to be applied to the fields of gas purification, sewage treatment and the like.
Description
Technical Field
The invention relates to a preparation method of high-performance activated carbon fibers, and belongs to the technical field of carbon fibers.
Background
Activated carbon fibers (ACFs for short) are a novel efficient adsorption material developed and gradually industrialized in the last 70 th century. Compared to traditional granular or powdered activated carbon, ACFs have unique properties: large specific surface area, high carbon content, narrow micropore distribution, large adsorption capacity, high adsorption and desorption speed and easy regeneration; easy to process, can make into fiber, paper, felt, cloth, etc.; has the characteristics of high strength, no pulverization, and no looseness or excessive compactness under the vibration condition. Therefore, the advent of ACFs has generated a great interest in scientists and entrepreneurs at home and abroad.
However, the current ACFs products are usually prepared by using a single chemical agent as an activating agent and adopting a batch activation method, and although the final ACFs have a high specific surface area, the ACFs samples prepared by the method have relatively low mechanical properties and cannot be used for forming products in various shapes, thereby limiting the application fields of the ACFs. Therefore, a new activation method is found to ensure that the ACFs sample has a certain specific surface area and also has important significance for endowing the ACFs sample with certain mechanical strength. The present invention utilizes existing activation equipment toAs variable, the specific surface area is 1500-2550 m by adopting a proper activation method2.g-1And a high-performance activated carbon fiber having a tensile strength of 0.5 to 0.9 GPa.
Disclosure of Invention
The purpose of the invention is as follows: intended to be assisted by existing activation equipment, toAs variable, ACFs products with high specific surface area and excellent mechanical properties are prepared by adopting a proper activation method, and finally the problems of low preparation efficiency, low cost and the like existing in the preparation of the existing adsorption material are solved,Low mechanical strength of the sample, high production cost and the like.
Another object of the present invention is to provide a use of the high-performance activated carbon fiber.
The purpose of the invention is realized by the following measures:
a preparation method of high-performance activated carbon fiber is characterized in that a single physical activation method or a physical-chemical synergistic activation method is adopted.
The method for preparing the high-performance activated carbon fiber by the single physical activation method comprises the steps of activating pre-oxidized carbon fiber by adopting continuous activation equipment, introducing water vapor and inert gas into the equipment, wherein the activation temperature is 700-900 ℃, and preferably 800-875 ℃; the activation time is 10-40 min, preferably 20-30 min,expressed as VSteam of water：(VSteam of water+VInert gas) The control is realized by adjusting the gas flow meter,a value of 0.4 × 10-4～4.5×10-4(ii) a V for every 6.5L volume of equipmentSteam of waterAt a flow rate of 1.04 × 10-4L.min-1。
The method for preparing the high-performance activated carbon fiber by the physical-chemical synergistic activation method comprises the steps of dipping pre-oxidized carbon fiber into an activator solution, activating the fiber dipped with the activator by using continuous activation equipment, and introducing water vapor and inert gas into the equipment, wherein the activation temperature is 700-900 ℃, and preferably 800-875 ℃; the activation time is 10-40 min, preferably 20-30 min,expressed as VSteam of water：(VSteam of water+VInert gas) The control is realized by adjusting the gas flow meter,a value of 0.4 × 10-4～4.5×10-4(ii) a V for every 6.5L volume of equipmentSteam of waterAt a flow rate of 1.04 × 10-4L.min-1The activation of the fiber is promoted by means of an activating agent and water vapor synergistic activation method. After the washing is finished, the obtained sample is repeatedly washed by distilled water, then boiled by the distilled water, and finally repeatedly washed by the distilled water until the washed solution is neutral.
Preparing pre-oxidized carbon fibers: the fiber raw material is pre-oxidized, the pre-oxidation temperature zone is (180-277 ℃), the pre-oxidation atmosphere is air atmosphere, and the total time of the fiber staying in the pre-oxidation furnace is 50-80 min.
The fiber raw material is selected from polyacrylonitrile-based, asphalt-based, viscose-based and phenolic-based fibers, and various forms of products such as felts, cloths and belts formed by the fibers. Wherein, the polyacrylonitrile-based fiber can be spun by a wet spinning method, a dry spinning method or a dry-jet wet spinning method, and the fiber tow can be 1-320K;
the copolymer of one or more monomers with the mass fraction of less than 10 percent in the polyacrylonitrile-based fiber is as follows: itaconic acid, methyl acrylate, acrylic acid, allyl chloride, alpha-chloropropene, methacrylic acid, methyl methacrylate, hydroxyalkyl acrylonitrile, hydroxyalkyl acrylic acid and esters thereof, acrylamide, methacrylamide, diacetone acrylamide, methacrylacetone, and the like. In particular, the different comonomers are added during the copolymerization of the acrylonitrile, and the invention can be applicable as long as the mass fraction of the acrylonitrile monomer in the polyacrylonitrile protofilament is higher than 90 percent.
On an existing activation equipment, toAs variables, the high-performance activated carbon fiber with high specific surface area and excellent tensile strength is prepared by adopting a proper activation method. Wherein,can be expressed as VSteam of water：(VSteam of water+VInert gas) The control is realized by adjusting the gas flow meter,a value of 0.4 × 10-4～4.5×10-4。
The activation equipment comprises batch activation equipment and continuous activation equipment.
Said variables beingThe regulation and control are carried out by a gas flowmeter.
The activator is selected from sodium hydroxide, potassium hydroxide, zinc chloride, K3PO4The mass percentage concentration of the activating agent is 9-20%.
The activation method covers a single physical activation method and a physical-chemical synergistic activation method.
The specific surface area of the active carbon fiber prepared by the method is 1500-2550 m2.g-1The tensile strength is 0.5-0.9 GPa.
The principle of the invention is as follows: in the process of preparing the high-performance activated carbon fiber by adopting a single physical activation method and a physical-chemical synergistic activation method, the change of the gas flow in the system can influence the systemTo affect the relevant properties of the final article.
The invention has the beneficial effects that: in the volume fraction of water vapourIn the process of regulating and controlling the adsorption property and the mechanical property of the sample for variables, the method can be used for controlling the adsorption property and the mechanical property of the sampleThe value is 0.4 × 10-4～4.5×10-4When the specific surface area is within the range, the specific surface area of the product is 1500-2550 m2.g-1The tensile strength is 0.5-0.9 GPa. The obtained carbon fiber can be used in the fields of gas purification, sewage treatment and the like, and the method adopted by the invention is simple, high in preparation efficiency and low in cost.
Drawings
FIG. 1 is a plot of specific surface area as a function of water vapor volume fraction for ACFs articles prepared in example 1 of the present invention;
FIG. 2 is a plot of tensile strength per filament as a function of water vapor volume fraction for ACFs articles made in example 1 of the present invention.
Detailed Description
The following further describes particular embodiments of the present invention to facilitate further understanding of the present invention by those skilled in the art, and does not constitute a limitation to the right thereof.
Example 1: the preparation method of the high-performance activated carbon fiber according to the embodiment is specifically carried out according to the following steps:
firstly, carrying out a pre-oxidation process on 12K PAN protofilament in a six-temperature-zone continuous pre-oxidation furnace (the pre-oxidation temperature zone is 180-277 ℃), wherein the pre-oxidation atmosphere is an air atmosphere, and the total time of the fiber staying in the pre-oxidation furnace is 70 min.
Secondly, using the pre-oxidized fiber obtained under the conditions as a precursor, firstly soaking the precursor fiber into a KOH solution with the mass fraction of 9%, and then activating the fiber soaked with an activating agent by using continuous activation equipment (the volume is 6.5L) (the activation temperature and the activation time are respectively 850℃)20 min.) at the same time, 1.04 × 10 g of water vapor was added with nitrogen-4L.min-1The flow rate of the activating agent is transmitted to an activating furnace from the outside, and the purpose of promoting the activation of the fibers is achieved by means of a KOH + water vapor synergistic activation method.
Thirdly, by regulating and controlling the flow of the nitrogen gasAdjusted to 0.4 × 10 in turn-4、1.5×10-4、2.5×10-4、3.5×10-4And 4.5 × 10-4After the experiment is finished, the obtained sample is repeatedly washed by distilled water, then is put into a beaker to be boiled, and finally is repeatedly washed by the distilled water until the washed solution is neutral.
And fourthly, respectively carrying out characterization on the relevant adsorption performance and the mechanical strength of the obtained ACFs product.
Example 2: this embodiment differs from example 1 in that: in the first step, 24K PAN precursor was used as a raw material, and the rest was the same as in example 1. The specific surface area of the ACFs product is 1450-2270 m2.g-1The tensile strength is 0.7 to 1.0 GPa.
Example 3: this embodiment differs from embodiment 1 in that: in the first step, a pre-oxidation device is adopted as a four-temperature-zone continuous pre-oxidation furnace, the residence time of the fiber in each temperature zone is 20min, and the rest is the same as that of the embodiment 1. The specific surface areas of the ACFs were 1390m each2.g-1、1562m2.g-1、1731m2.g-1、1947m2.g-1And 2160m2.g-1The corresponding tensile strengths of the filaments were 1.03GPa, 0.89GPa, 0.76GPa, 0.69GPa and 0.74 GPa.
Example 4: this embodiment differs from example 1 in that: will be in the third stepAdjusted to 0.27 × 10 in turn-4、1.0×10-4、1.67×10-4、2.33×10-4And 3.0 × 10-4Otherwise, the same as in example 1. The specific surface area of the ACFs product is 1153-2071 m2.g-1The tensile strength is 0.8 to 1.1 GPa.
Example 5: this embodiment differs from examples 1 to 4 in that: the activation time of the sample in step two was 10min, and the rest was the same as in example 1. The specific surface area of the ACFs product is 1021-1830 m2.g-1The tensile strength is 0.7 to 1.2 GPa.
Example 6: this embodiment differs from examples 1 to 5 in that: step two adopts K3PO4+ steam co-activation method, K3PO415 percent of,Adjusted to 0.67 × 10 in turn-4、2.5×10-4、4.17×10-4、5.83×10-4And 7.5 × 10-4Otherwise, the same as in example 1. The specific surface areas of the ACFs were 702m each2.g-1、820m2.g-1、897m2.g-1、961m2.g-1And 1040m2.g-1The corresponding tensile strengths of the filaments were 1.24GPa, 1.07GPa, 0.93GPa, 0.89GPa and 0.81 GPa.
Example 7: the embodiment is different from the embodiment in that: in step two, K3PO4The mass fraction was 9%, and others were the same as in example 1. The specific surface area of the ACFs product is 670-980 m2.g-1The tensile strength is 0.8 to 1.3 GPa.
Example 8: this embodiment differs from example 1 in that: in step two, K3PO4The mass fraction was 9%, the activation temperature was 900 ℃ and the other steps were the same as in example 1. The specific surface area of the ACFs product is 755-1050 m2.g-1The tensile strength is 0.7 to 1.2 GPa.
Example 9: this embodiment differs from embodiment 1 in that: in the second step, a single steam activation method is adopted,adjusted to 5.3 × 10 in turn-4、20×10-4、33.3×10-4、46.7×10-4And 60 × 10-4Otherwise, the same as in embodiment 1. The specific surface areas of the ACFs were 450m each2.g-1、572m2.g-1、702m2.g-1、804m2.g-1And 820m2.g-1The corresponding tensile strengths of the filaments were 1.30GPa, 1.22GPa, 1.01GPa, 0.86GPa and 0.71 GPa.
Example 10: this embodiment differs from embodiment 1 in that: in the second step, a single steam activation method is adopted,in turn adjusted to 8 × 10-4、30×10-4、50×10-4、70×10-4And 90 × 10-4The activation temperature was 900 ℃ and the other steps were the same as in example 1. The specific surface area of the ACFs product is 570-910 m2.g-1The tensile strength is 0.6 to 1.1 GPa.
Example 11: this embodiment differs from embodiment 1 in that: the inert gas used in step three was argon, otherwise as in example 1. The specific surface area of the ACFs product is 1530-2560 m2.g-1The tensile strength is 0.6-0.8 GPa.
Claims (6)
1. A preparation method of high-performance activated carbon fiber is characterized in that a single physical activation method or a physical-chemical synergistic activation method is adopted;
the method for preparing the high-performance activated carbon fiber by the single physical activation method comprises the steps of activating pre-oxidized carbon fiber by adopting continuous activation equipment, introducing water vapor and inert gas into the equipment, wherein the activation temperature is 700-900 ℃; the activation time is 10-40 min, expressed as VSteam of water：(VSteam of water+VInert gas) The control is realized by adjusting the gas flow meter,a value of 0.4 × 10-4～4.5×10-4；
The method for preparing the high-performance activated carbon fiber by the physical-chemical synergistic activation method comprises the steps of dipping pre-oxidized carbon fiber into an activator solution, activating the fiber dipped with the activator by using continuous activation equipment, and introducing water vapor and inert gas into the equipment, wherein the activation temperature is 700-900 ℃; the activation time is 10-40 min,expressed as VSteam of water：(VSteam of water+VInert gas) The control is realized by adjusting the gas flow meter,a value of 0.4 × 10-4～4.5×10-4(ii) a The purpose of promoting the activation of the fibers is achieved by means of an activating agent and water vapor synergistic activation method; after the washing is finished, the obtained sample is repeatedly washed by distilled water, then boiled by the distilled water, and finally repeatedly washed by the distilled water until the washed solution is neutral.
2. The method according to claim 1, wherein the activation temperature of the single physical activation method or the physical-chemical synergistic activation method is 800 to 875 ℃ and the activation time is 20 to 30 min.
3. A method according to claim 1, characterized in that the single physical activation method or the physical-chemical co-activation method corresponds to V per 6.5L volume of the apparatusSteam of waterAt a flow rate of1.04×10-4L.min-1。
4. The method according to claim 1, characterized in that the preparation of the pre-oxidized carbon fibers: the fiber raw material is pre-oxidized, the pre-oxidation temperature zone is 180-277 ℃, the pre-oxidation atmosphere is air atmosphere, and the total time of the fiber staying in the pre-oxidation furnace is 50-80 min.
5. A method according to claim 4, characterized in that the raw fibre material is selected from the group consisting of polyacrylonitrile-based, pitch-based, viscose-based and phenolic-based fibres, and articles formed therefrom in various forms; wherein the polyacrylonitrile-based fiber is spun by a wet spinning method, a dry spinning method or a dry-jet wet spinning method, and the fiber tow is 1-320K;
the polyacrylonitrile-based fiber also comprises a copolymer of one or more monomers with the mass fraction of less than 10 percent: itaconic acid, methyl acrylate, acrylic acid, allyl chloride, alpha-chloropropene, methacrylic acid, methyl methacrylate, hydroxyalkyl acrylonitrile, hydroxyalkyl acrylic acid and esters thereof, acrylamide, methacrylamide, diacetone acrylamide, methacrylacetone; in particular, the above-mentioned different comonomers are added during the copolymerization of acrylonitrile.
6. A process according to claim 1, characterized in that the activator is selected from the group consisting of sodium hydroxide, potassium hydroxide, zinc chloride, K3PO4The mass percentage concentration of the activating agent is 9-20%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109082880A (en) * | 2018-07-05 | 2018-12-25 | 王伟霞 | Functional activity carbon fiber, preparation method and applications |
| CN111135793A (en) * | 2020-01-07 | 2020-05-12 | 江苏竹海活性炭有限公司 | Renewable efficient deep desulfurization activated carbon and preparation method and application thereof |
| CN115142258A (en) * | 2022-06-24 | 2022-10-04 | 北京化工大学常州先进材料研究院 | High-efficiency preparation method of PAN-based activated carbon fiber felt |
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| JP2003138433A (en) * | 2001-10-30 | 2003-05-14 | Mitsubishi Heavy Ind Ltd | Method for producing active carbon fiber for flue gas desulfurization |
| CN101337176A (en) * | 2008-08-08 | 2009-01-07 | 东华大学 | Preparation method of macropore activated carbon fiber with intensity more than 0.3GPa |
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