CN113913969A - Method for preparing hydrophobic activated carbon fiber from carbon felt leftover material - Google Patents
Method for preparing hydrophobic activated carbon fiber from carbon felt leftover material Download PDFInfo
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- CN113913969A CN113913969A CN202111369016.6A CN202111369016A CN113913969A CN 113913969 A CN113913969 A CN 113913969A CN 202111369016 A CN202111369016 A CN 202111369016A CN 113913969 A CN113913969 A CN 113913969A
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- carbon felt
- felt leftover
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 134
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 108
- 239000000463 material Substances 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 41
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 34
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000005507 spraying Methods 0.000 claims abstract description 45
- 230000004913 activation Effects 0.000 claims abstract description 37
- 230000003213 activating effect Effects 0.000 claims abstract description 27
- 238000003763 carbonization Methods 0.000 claims abstract description 19
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 238000007689 inspection Methods 0.000 claims abstract description 9
- 238000005070 sampling Methods 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 27
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000011084 recovery Methods 0.000 claims description 10
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000012266 salt solution Substances 0.000 claims description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 4
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 2
- 239000001099 ammonium carbonate Substances 0.000 claims description 2
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 2
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 2
- 229910021538 borax Inorganic materials 0.000 claims description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 2
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 2
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 2
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 2
- 235000011151 potassium sulphates Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 235000002639 sodium chloride Nutrition 0.000 claims description 2
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 2
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002912 waste gas Substances 0.000 abstract description 2
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 description 8
- 239000011148 porous material Substances 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000004917 carbon fiber Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 239000012190 activator Substances 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 239000002920 hazardous waste Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- -1 phenolic aldehyde Chemical class 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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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
-
- 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
- D01F11/122—Oxygen, oxygen-generating compounds
-
- 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
- D01F11/123—Oxides
Abstract
The invention provides a method for preparing hydrophobic activated carbon fibers from carbon felt leftover materials, which comprises the following steps: s1, pretreatment: cutting the carbon felt leftover into blocks; s2, laying a net: uniformly paving blocky carbon felt leftover materials on the upper surface of a conveying mesh belt; s3, spraying and presoaking on the front surface and the back surface: activating the upper surface and the lower surface of the conveying mesh belt by spraying an activating agent, and starting a negative pressure suction device in the conveying process of the conveying mesh belt; s4, steam activation: processing the carbon felt leftover material by steam; s5, carbonization and activation: putting the carbon felt leftover materials into a carbonization furnace for further activation; s6, performing selective inspection and boxing: sampling and inspecting the carbon felt leftover material, wherein when the specific surface area of the processed carbon felt leftover material is larger than 1200m2And the/g is qualified product, and the unqualified product is recycled until the unqualified product is changed into qualified product. The method for preparing the hydrophobic activated carbon fiber from the carbon felt leftover material obtains the hydrophobic activated carbon fiber with huge specific surface area and widely distributed micropore structure, and the applicationIn the industries of waste gas treatment, waste water treatment and the like.
Description
Technical Field
The invention relates to the technical field of carbon fibers, in particular to a method for preparing hydrophobic activated carbon fibers from carbon felt leftover materials.
Background
The activated carbon fiber is activated carbon-containing fiber, and certain carbon-containing fiber (such as phenolic aldehyde-based fiber, PAN-based fiber, viscose-based fiber, asphalt-based fiber and the like) is activated at high temperature (different activation temperatures of different activation methods) to generate nanoscale pore diameters on the surface of the carbon-containing fiber, so that the specific surface area is increased, and the physical and chemical properties of the carbon-containing fiber are changed.
The activated carbon fiber has a large specific surface area (1000-3000 m)2/g) and abundant micropores, the micropore volume accounting for more than 90% of the total pore volume. The active carbon fiber has larger adsorption capacity and faster adsorption dynamic performance than granular active carbon, has high adsorption efficiency to organic matters and anions and cations in liquid phase and gas phase, has high adsorption and desorption speeds, can be regenerated and recycled, is acid-resistant, alkali-resistant, high-temperature-resistant, strong adaptability and good conductivity and chemical stability, is an ideal environment-friendly material, can selectively adsorb pollutant in gas or water solution, and has better regenerability after being used, so that the ACF (active carbon fiber) and deep-processed products thereof are widely applied to the field of environmental purification, and are widely applied to the recovery of purified gas, water and organic solvent at present.
In actual production, after the carbon felt product is cut according to the size and the shape required by a customer, the cut leftover materials are generally about 5% of the output, and are mostly taken as wastes to be recycled by qualified units, so that not only is a large amount of waste of production enterprises caused, but also the wastes are taken as hazardous wastes to cause great environmental pressure on hazardous waste treatment units.
Therefore, how to effectively treat, recycle and reuse the leftover materials of the carbon felt products is not only a technical subject of saving cost and reducing consumption of production enterprises, but also a requirement of environmental protection.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a method for preparing hydrophobic activated carbon fibers from carbon felt leftover materials. The technical scheme adopted by the invention is as follows:
a method for preparing hydrophobic activated carbon fibers from carbon felt leftover materials comprises the following steps:
s1, pretreatment: cutting the carbon felt leftover materials into blocks with the size of 5-10 cm;
s2, laying a net: uniformly paving blocky carbon felt leftover materials on the upper surface of a conveying mesh belt;
s3, spraying and presoaking on the front surface and the back surface: activating by spraying an activating agent on the upper surface and the lower surface of the conveying mesh belt, arranging a negative pressure suction device and a solution recovery device below the conveying mesh belt, and starting the negative pressure suction device in the conveying process of the conveying mesh belt;
activation principle of activator: the content of alkali and alkaline earth metal elements in the carbon fiber has a great influence on the oxidation performance of the carbon fiber, and particularly, the oxidation catalyst of which the metal elements such as sodium are carbon can accelerate the speed of thermal oxidation. After the activating agent is added, in the subsequent carbonization stage, the oxygen content in the nitrogen atmosphere is controlled to be a certain concentration, so that part of C on the surface of the product can be oxidized to form CO or CO2And the like, so that the surface of the material has rich micropore structures.
S4, steam activation: treating the carbon felt leftover materials treated in the step S3 through steam so that an activating agent can be diffused into the carbon felt along with the steam;
s5, carbonization and activation: putting the carbon felt leftover processed in the step S4 into a carbonization furnace, and further activating in a nitrogen atmosphere;
s6, performing selective inspection and boxing: sampling the carbon felt leftover material processed in the step S5, and when the specific surface area of the processed carbon felt leftover material is more than 1200m2And the/g is qualified product, and the unqualified product is recycled from S2 to S6 until the unqualified product is changed into qualified product.
Preferably, the method for preparing the hydrophobic activated carbon fiber from the carbon felt leftover material comprises the step S3, wherein the spraying pressure is 0.5-2.5 kg, the spraying temperature is room temperature-50 ℃, and the spraying residence time is 30-50 min.
Preferably, in the method for manufacturing the hydrophobic activated carbon fiber by using the carbon felt leftover material, the setting pressure of the negative pressure suction device in the step S3 is-0.005 to-0.01 Mpa.
Preferably, in the method for preparing the hydrophobic activated carbon fiber from the carbon felt leftover material, the activating agent in the step S3 is 0.5-1.2 wt% of alkali solution or salt solution.
Preferably, the method for preparing the hydrophobic activated carbon fiber by using the carbon felt leftover material is used, wherein the alkali solution is one or more of potassium hydroxide, sodium carbonate, sodium bicarbonate and ammonium bicarbonate solution.
Preferably, the method for preparing the hydrophobic activated carbon fiber by using the carbon felt leftover material comprises the step of preparing a salt solution by using a solvent, wherein the salt solution is one or more of sodium chloride, potassium chloride, sodium sulfate, potassium sulfate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, sodium borate and potassium dihydrogen phosphate solution.
Preferably, in the method for preparing the hydrophobic activated carbon fiber from the carbon felt leftover material, the temperature of the steam in the step S4 is 134-152 ℃, and the pressure is 3-5 kg.
Preferably, the method for preparing the hydrophobic activated carbon fiber from the carbon felt leftover material comprises the following steps of S5 activation: controlling the oxygen content at 50-300 ppm in the nitrogen atmosphere, raising the room temperature to 300 ℃ at a speed of 10 ℃/h, keeping the temperature constant for 30min, raising the temperature to 550 ℃ at a speed of 15-20 ℃/h, keeping the temperature constant for 30min, finally raising the temperature to 750 ℃ at a speed of 15-20 ℃/h, keeping the temperature constant for 30-50 min, continuously introducing nitrogen, cooling to the room temperature, and taking out.
The invention has the advantages that:
(1) according to the method for preparing the hydrophobic activated carbon fiber by using the carbon felt leftover material, the carbon felt leftover material is subjected to front and back spraying and presoaking, steam activation and carbonization activation treatment in sequence, so that the hydrophobic activated carbon fiber with a huge specific surface area and a widely distributed microporous structure can be obtained, the method is applied to industries such as waste gas treatment, waste water treatment and the like, huge economic benefits and environmental benefits are generated, and the original dangerous waste is changed into an environment-friendly product.
(2) The method for preparing the hydrophobic activated carbon fiber by the carbon felt leftover materials comprises the steps of spraying and pre-dipping the carbon felt leftover materials from the front side and the back side, arranging the negative pressure suction device and the redundant solution recovery device below the conveying belt, and enhancing the effect of the activating agent in the carbon felt leftover materialsThe diffusion and the permeation of the activator are reduced, and the use amount of the activator is saved; activating the carbon felt leftover materials through steam, so that an activating agent can enter the carbon felt along with the diffusion of the steam, and further enhancing the diffusion and permeation of the carbon felt leftover materials; carbonizing and activating the carbon felt leftover materials to further activate the carbon felt leftover materials, and finally obtaining the carbon felt leftover materials with the specific surface area of more than 1200m2And/g, the hydrophobic activated carbon fiber has a microporous structure with more than 90% of pore structure and a micropore size and a pore diameter of 1.0-3.0 nm.
Drawings
FIG. 1 is a flow chart of a method for preparing hydrophobic activated carbon fibers from carbon felt leftover materials.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
A method for preparing hydrophobic activated carbon fibers from carbon felt leftover materials comprises the following steps:
s1, pretreatment: cutting the carbon felt leftover materials into blocks with the size of 5-10 cm;
s2, laying a net: uniformly paving blocky carbon felt leftover materials on the upper surface of a conveying mesh belt;
s3, spraying and presoaking on the front surface and the back surface: spraying 1wt% of sodium hydroxide solution on the upper surface and the lower surface of a conveying mesh belt for activation, wherein the spraying pressure is 0.5kg, the spraying temperature is room temperature, the spraying retention time is 50min, a negative pressure suction device and a solution recovery device are arranged below the conveying mesh belt, the negative pressure suction device is started in the conveying process of the conveying mesh belt, and the setting pressure of the negative pressure suction device is-0.005 Mpa;
s4, steam activation: treating the carbon felt leftover processed in the step S3 by steam, wherein the temperature of the steam is 134 ℃, and the pressure of the steam is 3kg, so that an activating agent can diffuse into the carbon felt along with the steam;
s5, carbonization and activation: and (4) putting the carbon felt leftover materials processed in the step (S4) into a carbonization furnace, and further activating in a nitrogen atmosphere, wherein the activation specifically comprises the following steps: under the nitrogen atmosphere, controlling the oxygen content to be about 100ppm, raising the room temperature to 300 ℃ at a speed of 10 ℃/h, keeping the temperature constant for 30min, raising the temperature to 550 ℃ at a speed of 15-20 ℃/h, keeping the temperature constant for 30min, finally raising the temperature to 750 ℃ at a speed of 15-20 ℃/h, keeping the temperature constant for 30min, continuously introducing nitrogen, cooling to the room temperature, and taking out;
s6, performing selective inspection and boxing: sampling the carbon felt leftover material processed in the step S5, and when the specific surface area of the processed carbon felt leftover material is more than 1200m2And the/g is qualified products, and the unqualified products are boxed, and the steps from S2 to S6 are repeated until the unqualified products become qualified products.
Example 2
A method for preparing hydrophobic activated carbon fibers from carbon felt leftover materials comprises the following steps:
s1, pretreatment: cutting the carbon felt leftover materials into blocks with the size of 5-10 cm;
s2, laying a net: uniformly paving blocky carbon felt leftover materials on the upper surface of a conveying mesh belt;
s3, spraying and presoaking on the front surface and the back surface: spraying 0.8wt% sodium bicarbonate solution on the upper and lower surfaces of the conveying mesh belt for activation, wherein the spraying pressure is 1kg, the spraying temperature is 35 ℃ at room temperature, the spraying residence time is 40min,
a negative pressure suction device and a solution recovery device are arranged below the conveying belt, the negative pressure suction device is started in the conveying process of the conveying belt, and the set pressure of the negative pressure suction device is-0.008 Mpa;
s4, steam activation: treating the carbon felt leftover processed in the step S3 by steam, wherein the temperature of the steam is 142 ℃, and the pressure of the steam is 4kg, so that an activating agent can diffuse into the carbon felt along with the steam;
s5, carbonization and activation: and (4) putting the carbon felt leftover materials processed in the step (S4) into a carbonization furnace, and further activating in a nitrogen atmosphere, wherein the activation specifically comprises the following steps: under the nitrogen atmosphere, controlling the oxygen content to be about 150ppm, raising the room temperature to 300 ℃ at a speed of 10 ℃/h, keeping the temperature constant for 30min, raising the temperature to 550 ℃ at a speed of 15-20 ℃/h, keeping the temperature constant for 30min, finally raising the temperature to 750 ℃ at a speed of 15-20 ℃/h, keeping the temperature constant for 40min, continuously introducing nitrogen, cooling to the room temperature, and taking out;
s6, performing selective inspection and boxing: sampling the carbon felt leftover material processed in the step S5, and when the specific surface area of the processed carbon felt leftover material is more than 1200m2The/g is qualified products and boxed, and the unqualified products are recycled from S2 to S6 until the qualified products are qualifiedAnd (5) preparing the product.
Example 3
A method for preparing hydrophobic activated carbon fibers from carbon felt leftover materials comprises the following steps:
s1, pretreatment: cutting the carbon felt leftover materials into blocks with the size of 5-10 cm;
s2, laying a net: uniformly paving blocky carbon felt leftover materials on the upper surface of a conveying mesh belt;
s3, spraying and presoaking on the front surface and the back surface: spraying 1.2wt% of sodium sulfate solution on the upper surface and the lower surface of a conveying mesh belt for activation, wherein the spraying pressure is 2.5kg, the spraying temperature is 50 ℃, the spraying residence time is 30-50 min, a negative pressure suction device and a solution recovery device are arranged below the conveying mesh belt, the negative pressure suction device is started in the conveying process of the conveying mesh belt, and the setting pressure of the negative pressure suction device is-0.01 Mpa;
s4, steam activation: treating the carbon felt leftover processed in the step S3 by steam, wherein the temperature of the steam is 152 ℃, and the pressure of the steam is 5kg, so that an activating agent can diffuse into the carbon felt along with the steam;
s5, carbonization and activation: and (4) putting the carbon felt leftover materials processed in the step (S4) into a carbonization furnace, and further activating in a nitrogen atmosphere, wherein the activation specifically comprises the following steps: under the nitrogen atmosphere, controlling the oxygen content to be about 200ppm, raising the room temperature to 300 ℃ at a speed of 10 ℃/h, keeping the temperature for 30min, raising the temperature to 550 ℃ at a speed of 15-20 ℃/h, keeping the temperature for 30min, finally raising the temperature to 750 ℃ at a speed of 15-20 ℃/h, keeping the temperature for 50min, continuously introducing nitrogen, cooling to the room temperature, and taking out;
s6, performing selective inspection and boxing: sampling the carbon felt leftover material processed in the step S5, and when the specific surface area of the processed carbon felt leftover material is more than 1200m2And the/g is qualified products, and the unqualified products are boxed, and the steps from S2 to S6 are repeated until the unqualified products become qualified products.
Comparative example 1
A method for preparing hydrophobic activated carbon fibers from carbon felt leftover materials comprises the following steps:
s1, pretreatment: cutting the carbon felt leftover materials into blocks with the size of 5-10 cm;
s2, laying a net: uniformly paving blocky carbon felt leftover materials on the upper surface of a conveying mesh belt;
s3, spraying and presoaking on the front surface and the back surface: spraying 1wt% of sodium hydroxide solution on the upper surface and the lower surface of a conveying mesh belt for activation, wherein the spraying pressure is 0.5kg, the spraying temperature is room temperature, the spraying retention time is 50min, a negative pressure suction device and a solution recovery device are arranged below the conveying mesh belt, the negative pressure suction device is started in the conveying process of the conveying mesh belt, and the setting pressure of the negative pressure suction device is-0.005 Mpa;
s4, carbonization and activation: and (4) putting the carbon felt leftover materials processed in the step (S3) into a carbonization furnace, and further activating in a nitrogen atmosphere, wherein the activation specifically comprises the following steps: under the nitrogen atmosphere, controlling the oxygen content to be about 100ppm, raising the room temperature to 300 ℃ at a speed of 10 ℃/h, keeping the temperature constant for 30min, raising the temperature to 550 ℃ at a speed of 15-20 ℃/h, keeping the temperature constant for 30min, finally raising the temperature to 750 ℃ at a speed of 15-20 ℃/h, keeping the temperature constant for 30min, continuously introducing nitrogen, cooling to the room temperature, and taking out;
s5, performing selective inspection and boxing: sampling the carbon felt leftover material processed in the step S4, and when the specific surface area of the processed carbon felt leftover material is more than 1200m2And the/g is qualified products, and the unqualified products are boxed, and the steps from S2 to S6 are repeated until the unqualified products become qualified products.
Comparative example 2
A method for preparing hydrophobic activated carbon fibers from carbon felt leftover materials comprises the following steps:
s1, pretreatment: cutting the carbon felt leftover materials into blocks with the size of 5-10 cm;
s2, laying a net: uniformly paving blocky carbon felt leftover materials on the upper surface of a conveying mesh belt;
s3, spraying and presoaking on the front surface and the back surface: spraying 0.8wt% sodium bicarbonate solution on the upper and lower surfaces of the conveying mesh belt for activation, wherein the spraying pressure is 1kg, the spraying temperature is 35 ℃ at room temperature, the spraying residence time is 40min,
a negative pressure suction device and a solution recovery device are arranged below the conveying belt, the negative pressure suction device is started in the conveying process of the conveying belt, and the set pressure of the negative pressure suction device is-0.008 Mpa;
s4, steam activation: treating the carbon felt leftover processed in the step S3 by steam, wherein the temperature of the steam is 142 ℃, and the pressure of the steam is 4kg, so that an activating agent can diffuse into the carbon felt along with the steam;
s5, performing selective inspection and boxing: sampling the carbon felt leftover material processed in the step S4, and when the specific surface area of the processed carbon felt leftover material is more than 1200m2And the/g is qualified products, and the unqualified products are boxed, and the steps from S2 to S6 are repeated until the unqualified products become qualified products.
Comparative example 3
A method for preparing hydrophobic activated carbon fibers from carbon felt leftover materials comprises the following steps:
s1, pretreatment: cutting the carbon felt leftover materials into blocks with the size of 5-10 cm;
s2, laying a net: uniformly paving blocky carbon felt leftover materials on the upper surface of a conveying mesh belt;
s3, spraying and presoaking on the front surface and the back surface: spraying 1.2wt% of sodium sulfate solution on the upper surface and the lower surface of the conveying mesh belt for activation, wherein the spraying pressure is 2.5kg, the spraying temperature is 50 ℃, the spraying residence time is 30-50 min, and a solution recovery device is arranged below the conveying mesh belt;
s4, steam activation: treating the carbon felt leftover processed in the step S3 by steam, wherein the temperature of the steam is 152 ℃, and the pressure of the steam is 5kg, so that an activating agent can diffuse into the carbon felt along with the steam;
s5, carbonization and activation: and (4) putting the carbon felt leftover materials processed in the step (S4) into a carbonization furnace, and further activating in a nitrogen atmosphere, wherein the activation specifically comprises the following steps: under the nitrogen atmosphere, controlling the oxygen content at 200ppm, raising the room temperature to 300 ℃ at a speed of 10 ℃/h, keeping the temperature constant for 30min, raising the temperature to 550 ℃ at a speed of 15-20 ℃/h, keeping the temperature constant for 30min, finally raising the temperature to 750 ℃ at a speed of 15-20 ℃/h, keeping the temperature constant for 50min, continuously introducing nitrogen, cooling to the room temperature, and taking out;
s6, performing selective inspection and boxing: sampling the carbon felt leftover material processed in the step S5, and when the specific surface area of the processed carbon felt leftover material is more than 1200m2And the/g is qualified products, and the unqualified products are boxed, and the steps from S2 to S6 are repeated until the unqualified products become qualified products.
The results of the performance tests of examples 1 to 3 and comparative examples 1 to 3 are shown below in Table 1.
TABLE 1
As can be seen from Table 1, after the carbon felt leftover materials of the embodiments 1 to 3 are subjected to spraying pre-dipping, steam activation and carbonization activation, the specific surface area is larger than 1200m2/g, more than 90% of the pore structure is a microporous structure, the pore size and the pore diameter are 1.0 to 3.0nm, and the specific surface area and the pore structure of the carbon felt leftover materials of the embodiments 1 to 3 are better than those of the comparative examples 1 to 3.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to examples, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (8)
1. A method for preparing hydrophobic activated carbon fibers from carbon felt leftover materials is characterized by comprising the following steps:
s1, pretreatment: cutting the carbon felt leftover materials into blocks with the size of 5-10 cm;
s2, laying a net: uniformly paving blocky carbon felt leftover materials on the upper surface of a conveying mesh belt;
s3, spraying and presoaking on the front surface and the back surface: activating by spraying an activating agent on the upper surface and the lower surface of the conveying mesh belt, arranging a negative pressure suction device and a solution recovery device below the conveying mesh belt, and starting the negative pressure suction device in the conveying process of the conveying mesh belt;
s4, steam activation: treating the carbon felt leftover materials treated in the step S3 through steam so that an activating agent can be diffused into the carbon felt along with the steam;
s5, carbonization and activation: putting the carbon felt leftover processed in the step S4 into a carbonization furnace, and further activating in a nitrogen atmosphere;
s6, performing selective inspection and boxing: sampling the carbon felt leftover material processed in the step S5, and when the specific surface area of the processed carbon felt leftover material is more than 1200m2And the/g is qualified product, and the unqualified product is recycled from S2 to S6 until the unqualified product is changed into qualified product.
2. The method for preparing the hydrophobic activated carbon fiber from the carbon felt leftover material according to claim 1, wherein the spraying pressure in the step S3 is 0.5-2.5 kg, the spraying temperature is room temperature-50 ℃, and the spraying residence time is 30-50 min.
3. The method for manufacturing the hydrophobic activated carbon fiber from the carbon felt leftover material according to claim 1, wherein the setting pressure of the negative pressure suction device in the step S3 is-0.005 MPa to-0.01 MPa.
4. The method for preparing the hydrophobic activated carbon fiber from the carbon felt leftover material according to claim 1, wherein the activating agent in the step S3 is 0.5-1.2 wt% of alkali solution or salt solution.
5. The method for preparing hydrophobic activated carbon fiber from carbon felt scraps as claimed in claim 4, wherein the alkali solution is one or more of potassium hydroxide, sodium carbonate, sodium bicarbonate and ammonium bicarbonate solution.
6. The method for manufacturing the hydrophobic activated carbon fiber from the carbon felt leftover material according to claim 4, wherein the salt solution is one or more of sodium chloride, potassium chloride, sodium sulfate, potassium sulfate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, sodium borate and potassium dihydrogen phosphate solution.
7. The method for preparing the hydrophobic activated carbon fiber from the carbon felt leftover material according to claim 1, wherein the temperature of the steam in the step S4 is 134-152 ℃, and the pressure is 3-5 kg.
8. The method for preparing the hydrophobic activated carbon fiber from the carbon felt leftover material according to claim 1, wherein the activation of the step S5 specifically comprises: controlling the oxygen content at 50-300 ppm in the nitrogen atmosphere, raising the room temperature to 300 ℃ at a speed of 10 ℃/h, keeping the temperature constant for 30min, raising the temperature to 550 ℃ at a speed of 15-20 ℃/h, keeping the temperature constant for 30min, finally raising the temperature to 750 ℃ at a speed of 15-20 ℃/h, keeping the temperature constant for 30-50 min, continuously introducing nitrogen, cooling to the room temperature, and taking out.
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