WO2022016663A1 - Reaming method for activated carbon fiber - Google Patents

Reaming method for activated carbon fiber Download PDF

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Publication number
WO2022016663A1
WO2022016663A1 PCT/CN2020/112095 CN2020112095W WO2022016663A1 WO 2022016663 A1 WO2022016663 A1 WO 2022016663A1 CN 2020112095 W CN2020112095 W CN 2020112095W WO 2022016663 A1 WO2022016663 A1 WO 2022016663A1
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Prior art keywords
activated carbon
cleaning
drying
carbon fiber
modification
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PCT/CN2020/112095
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French (fr)
Chinese (zh)
Inventor
金珊珊
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苏州远浩新纺织科技有限公司
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Publication of WO2022016663A1 publication Critical patent/WO2022016663A1/en

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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J13/00—Heating or cooling the yarn, thread, cord, rope, or the like, not specific to any one of the processes provided for in this subclass
    • D02J13/001—Heating or cooling the yarn, thread, cord, rope, or the like, not specific to any one of the processes provided for in this subclass in a tube or vessel
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/49—Oxides or hydroxides of elements of Groups 8, 9,10 or 18 of the Periodic Table; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
    • D06M11/59—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with ammonia; with complexes of organic amines with inorganic substances
    • D06M11/60—Ammonia as a gas or in solution
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/144—Alcohols; Metal alcoholates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
    • D06M13/256—Sulfonated compounds esters thereof, e.g. sultones
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
    • D06M13/262—Sulfated compounds thiosulfates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/35—Heterocyclic compounds
    • D06M13/355—Heterocyclic compounds having six-membered heterocyclic rings
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/53—Polyethers
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/40—Fibres of carbon

Definitions

  • the invention relates to the technical field of fibers, in particular to a method for expanding the pores of activated carbon fibers.
  • Fiber refers to a substance composed of continuous or discontinuous filaments. In animals and plants, fibers play an important role in maintaining tissues. Fibers are widely used and can be woven into thin threads, thread ends and hemp ropes. When making paper or weaving felt It can also be woven into a fiber layer, and it is also commonly used to make other materials, and to form composite materials together with other materials.
  • Activated carbon fiber is a kind of fiber, but the existing activated carbon fiber has limited adsorption capacity. In order to improve its adsorption However, the existing hole expansion method has an unsatisfactory hole expansion effect, which reduces its market competitiveness and does not meet the interests of the enterprise itself. For this reason, we propose a hole expansion method for activated carbon fibers. .
  • the purpose of the present invention is to provide a method for expanding the pores of activated carbon fibers, so as to solve the problems raised in the above-mentioned background art.
  • a method for expanding the pores of activated carbon fibers includes the following steps: A. Impurity removal: the activated carbon fibers are sent into an electrostatic trash removal box for surface impurity removal treatment; B. The first cleaning: the activated carbon fibers after impurity removal are sent into the cleaning box for cleaning treatment; C. The first drying: The activated carbon fibers after cleaning are sent into the drying box for drying treatment; D. The first modification Properties: The dried activated carbon fibers are placed in magnesium powder to react for 30-70min, and the reaction temperature is 900-1300°C; E. Second cleaning: The first modified activated carbon fibers are sent into the cleaning box for Cleaning treatment; F.
  • Second drying send the cleaned activated carbon fibers into a drying box for drying;
  • Second modification place the dried activated carbon fibers in a tube furnace for high-temperature ammonia modification. Then put the modified activated carbon fiber in a tube furnace, continue to heat up to 300 °C at a certain heating rate in a nitrogen atmosphere, then switch to an ammonia atmosphere, and continue to heat up to 900-1100 °C, here Carry out high temperature modification under the temperature, and modification time 2-3h;
  • H cleaning for the third time: the activated carbon fiber after the second modification is sent into the cleaning box for cleaning treatment;
  • Soaking soak the dried activated carbon fibers in an ethanol solution, and add hydroxide to the ethanol solution as a pore-enlarging agent; K.
  • the third modification Properties continue to soak the soaked activated carbon fiber in the surfactant, and heat it for 2-4h under nitrogen protection, and the heating temperature is 300-500 °C, and then switch the nitrogen gas to a mixed gas of water vapor and carbon dioxide, and Continue to heat at 700-800 °C for 1-3h;
  • L the fourth cleaning: send the activated carbon fiber after the third modification into the cleaning box for cleaning;
  • M the fourth drying: the cleaned The activated carbon fibers are sent into a drying box for drying to obtain pore-enlarging activated carbon fibers.
  • the cleaning liquids in the steps B, F, H and L are all plasma water, and the cleaning methods are ultrasonic vibration cleaning.
  • the frequency of the ultrasonic waves is 60-80Hz, and the oscillation time is 40-80min.
  • the cleaning box is also provided with a heater, which is one of a high-frequency induction heater, an inner coil heater or an electrode heater, and the temperature of the heater is 50-70°C.
  • the hydroxide in the step J is ferric hydroxide, ferrous hydroxide, zinc hydroxide, magnesium hydroxide, cobalt hydroxide, sodium hydroxide, potassium hydroxide, barium hydroxide or lithium hydroxide a kind of.
  • step G it also includes nitrogen heating: program heating under the condition that nitrogen is continuously introduced, and calcining at a temperature range of 900-1100 °C for 2.5-4 h at a heating rate of 10-20 °C/min. .
  • the surfactant in the step K is one of cetyl pyridine chloride, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, Tween or Span.
  • the drying temperatures in the steps C, F, I and M are all 100-150° C., and the drying times are all 60-90 min.
  • the soaking temperatures in the steps J and K are both 80-100° C., and the soaking times are both 4-6 hours.
  • stirring is performed once every 30-60 minutes, and each stirring is 2-4 minutes.
  • the beneficial effects of the present invention are as follows: in the present invention, activated carbon fibers are modified in magnesium powder for the first time, and high-temperature ammonia and nitrogen are modified for the second time in a tube furnace. After being soaked in surfactant, the third modification is carried out in a mixed gas of nitrogen, water vapor and carbon dioxide, which can effectively improve the pore-enlarging effect of activated carbon fibers, and has no effect on the overall strength of activated carbon fibers, thus expanding its market. Competitiveness is in the interests of the enterprise itself.
  • a method for expanding the pores of activated carbon fibers which includes the following steps: A. Impurity removal: the activated carbon fibers are sent into an electrostatic trash removal box for surface impurity removal treatment; B. The first cleaning: the activated carbon fibers after removal of impurities are cleaned Send it into a cleaning box for cleaning treatment; C. Drying for the first time: send the cleaned activated carbon fiber into a drying box for drying treatment; D. First modification: place the dried activated carbon fiber on magnesium powder The middle reaction is 30-70min, and the reaction temperature is 900-1300 °C; E, the second cleaning: the activated carbon fiber after the first modification is sent into the cleaning box for cleaning; F, the second drying: the The cleaned activated carbon fibers are sent to a drying box for drying; G.
  • Second modification place the dried activated carbon fibers in a tube furnace for high-temperature ammonia modification, and then place the modified activated carbon fibers in a In the tube furnace, continue to heat up to 300°C at a certain heating rate in a nitrogen atmosphere, then switch to an ammonia atmosphere, continue to heat up to 900-1100°C, and perform high-temperature modification at this temperature, and the modification time is 2 -3h; H, cleaning for the third time: the activated carbon fiber after the second modification is sent into the cleaning box for cleaning treatment; 1, drying for the third time: the activated carbon fiber after cleaning is sent into the drying box for drying Treatment; J.
  • Soaking soak the dried activated carbon fibers in an ethanol solution, and add hydroxide to the ethanol solution as a pore-enlarging agent; K.
  • the third modification continue to soak the soaked activated carbon fibers on the surface
  • the active agent is heated under nitrogen protection for 2-4h, and the heating temperature is 300-500°C, then the nitrogen is switched to a mixed gas of water vapor and carbon dioxide, and the heating is continued at 700-800°C for 1-3h;
  • L the fourth cleaning: the activated carbon fiber after the third modification is sent into the cleaning box for cleaning treatment;
  • M the fourth drying: the activated carbon fiber after the cleaning is sent into the drying box for drying treatment to obtain Pore-enlarging activated carbon fibers.
  • the activated carbon fiber is modified for the first time in magnesium powder, the second modification is carried out with high temperature ammonia and nitrogen in a tube furnace, and finally soaked in a surfactant and then in a mixed gas of nitrogen, water vapor and carbon dioxide.
  • the third modification can effectively improve the pore-enlarging effect of the activated carbon fiber without affecting the overall strength of the activated carbon fiber, thereby expanding its market competitiveness and conforming to the interests of the enterprise itself.
  • the cleaning solutions in steps B, F, H and L are all plasma water, and the cleaning methods are ultrasonic vibration cleaning.
  • the frequency of the ultrasonic wave is 60-80Hz, and the oscillation time is 40-80min.
  • the cleaning box is also provided with
  • the heater is one of a high-frequency induction heater, an inner coil heater or an electrode heater, and the temperature of the heater is 50-70°C.
  • the hydroxide in step J is one of ferric hydroxide, ferrous hydroxide, zinc hydroxide, magnesium hydroxide, cobalt hydroxide, sodium hydroxide, potassium hydroxide, barium hydroxide or lithium hydroxide.
  • step G nitrogen heating is also included: the temperature is programmed under the condition that nitrogen is continuously introduced, and calcination is set at a temperature range of 900-1100 °C for 2.5-4 hours at a heating rate of 10-20 °C/min.
  • the surfactant in step K is a kind of in cetyl pyridine chloride, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, Tween or span.
  • drying temperatures in steps C, F, I and M are all 100-150° C., and the drying times are all 60-90 min.
  • the soaking temperatures in steps J and K are both 80-100° C., and the soaking times are both 4-6 h. At the same time, stirring is performed once at intervals of 30-60 minutes, and stirring is performed for 2-4 minutes each time.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Inorganic Fibers (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

Provided is a reaming method for an activated carbon fiber, comprising: A, impurity removal; B, primary cleaning; C, primary drying; D, primary modification: putting dried activated carbon fibers into magnesium powder to react for 30-70 min, the reaction temperature being 900-1300ºC; E, secondary cleaning; F, secondary drying; G, secondary modification: performing high-temperature ammonia modification, first heating up to 300ºC in a nitrogen atmosphere, switching to an ammonia atmosphere, continuing heating up to 900-1100ºC, and modifying for 2-3 h; H, third cleaning; I, third drying; J, soaking: soaking the dried activated carbon fibers in an ethanol solution, and adding hydroxide in the ethanol solution as a pore-enlarging agent; K, third modification: continuing soaking the activated carbon fibers in a surfactant, heating under nitrogen protection for 2-4 h with the heating temperature of 300-500ºC, then switching nitrogen to a mixed gas of water vapor and carbon dioxide, and heating at 700-800ºC for 1-3 h; L, fourth cleaning; and M, fourth drying, to obtain a reamed activated carbon fiber. The method can effectively improve the reaming effect of the activated carbon fiber, and does not affect the overall strength of activated carbon fiber.

Description

活性炭纤维的扩孔方法Pore expansion method of activated carbon fiber 技术领域technical field
本发明涉及纤维技术领域，具体为活性炭纤维的扩孔方法。The invention relates to the technical field of fibers, in particular to a method for expanding the pores of activated carbon fibers.
背景技术Background technique
纤维是指由连续或不连续的细丝组成的物质，在动植物体内，纤维在维系组织方面起到重要作用，纤维用途广泛，可织成细线、线头和麻绳，造纸或织毡时还可以织成纤维层，同时也常用来制造其他物料，及与其他物料共同组成复合材料，活性炭纤维是纤维中的一种，但现有的活性炭纤维其自身的吸附能力有限，为了提高其吸附效果，需要对其进行扩孔处理，但现有的扩孔方法其扩孔效果不理想，从而降低了其市场竞争力，不符合企业自身的利益，为此，我们提出活性炭纤维的扩孔方法。Fiber refers to a substance composed of continuous or discontinuous filaments. In animals and plants, fibers play an important role in maintaining tissues. Fibers are widely used and can be woven into thin threads, thread ends and hemp ropes. When making paper or weaving felt It can also be woven into a fiber layer, and it is also commonly used to make other materials, and to form composite materials together with other materials. Activated carbon fiber is a kind of fiber, but the existing activated carbon fiber has limited adsorption capacity. In order to improve its adsorption However, the existing hole expansion method has an unsatisfactory hole expansion effect, which reduces its market competitiveness and does not meet the interests of the enterprise itself. For this reason, we propose a hole expansion method for activated carbon fibers. .
技术解决方案technical solutions
本发明的目的在于提供活性炭纤维的扩孔方法，以解决上述背景技术中提出的问题。The purpose of the present invention is to provide a method for expanding the pores of activated carbon fibers, so as to solve the problems raised in the above-mentioned background art.
为实现上述目的，本发明提供如下技术方案：活性炭纤维的扩孔方法，其扩孔方法包括以下步骤：A、除杂：将活性炭纤维送入静电除杂箱内进行表面除杂处理；B、第一次清洗：将除杂后的活性炭纤维送入清洗箱内进行清洗处理；C、第一次烘干：将清洗后的活性炭纤维送入干燥箱内进行干燥处理；D、第一次改性：将干燥后的活性炭纤维置于镁粉中反应30-70min，且反应温度为900-1300℃；E、第二次清洗：将第一次改性后的活性炭纤维送入清洗箱内进行清洗处理；F、第二次烘干：将清洗后的活性炭纤维送入干燥箱内进行干燥处理；G、第二次改性：将干燥后活性炭纤维置于管式炉中进行高温氨气改性，然后将改性后的活性炭纤维置于管式炉中，继续在氮气气氛下以一定的升温速率升温至300℃，然后切换至氨气气氛下，继续升温至900-1100℃，在此温度下进行高温改性，且改性时间2-3h；H、第三次清洗：将第二次改性后的活性炭纤维送入清洗箱内进行清洗处理；I、第三次烘干：将清洗后的活性炭纤维送入干燥箱内进行干燥处理；J、浸泡：将干燥后的活性炭纤维浸泡于乙醇溶液中，并在乙醇溶液中加入氢氧化物为扩孔剂；K、第三次改性：将浸泡后的活性炭纤维继续浸泡在表面活性剂中，并在在氮气保护下加热2-4h，且加热温度为300-500℃，然后将氮气切换成水蒸气和二氧化碳的混合气体，并继续在700-800℃下加热1-3h；L、第四次清洗：将第三次改性后的活性炭纤维送入清洗箱内进行清洗处理；M、第四次烘干：将清洗后的活性炭纤维送入干燥箱内进行干燥处理，得到扩孔活性炭纤维。In order to achieve the above purpose, the present invention provides the following technical solutions: a method for expanding the pores of activated carbon fibers, and the method for expanding the pores includes the following steps: A. Impurity removal: the activated carbon fibers are sent into an electrostatic trash removal box for surface impurity removal treatment; B. The first cleaning: the activated carbon fibers after impurity removal are sent into the cleaning box for cleaning treatment; C. The first drying: The activated carbon fibers after cleaning are sent into the drying box for drying treatment; D. The first modification Properties: The dried activated carbon fibers are placed in magnesium powder to react for 30-70min, and the reaction temperature is 900-1300℃; E. Second cleaning: The first modified activated carbon fibers are sent into the cleaning box for Cleaning treatment; F. Second drying: send the cleaned activated carbon fibers into a drying box for drying; G. Second modification: place the dried activated carbon fibers in a tube furnace for high-temperature ammonia modification. Then put the modified activated carbon fiber in a tube furnace, continue to heat up to 300 ℃ at a certain heating rate in a nitrogen atmosphere, then switch to an ammonia atmosphere, and continue to heat up to 900-1100 ℃, here Carry out high temperature modification under the temperature, and modification time 2-3h; H, cleaning for the third time: the activated carbon fiber after the second modification is sent into the cleaning box for cleaning treatment; I, drying for the third time: the The cleaned activated carbon fibers are sent into the drying box for drying treatment; J. Soaking: soak the dried activated carbon fibers in an ethanol solution, and add hydroxide to the ethanol solution as a pore-enlarging agent; K. The third modification Properties: continue to soak the soaked activated carbon fiber in the surfactant, and heat it for 2-4h under nitrogen protection, and the heating temperature is 300-500 ℃, and then switch the nitrogen gas to a mixed gas of water vapor and carbon dioxide, and Continue to heat at 700-800 ℃ for 1-3h; L, the fourth cleaning: send the activated carbon fiber after the third modification into the cleaning box for cleaning; M, the fourth drying: the cleaned The activated carbon fibers are sent into a drying box for drying to obtain pore-enlarging activated carbon fibers.
优选的，所述步骤B、F、H和L中的清洗液均为等离子水，且清洗方式均为超声波震荡清洗，同时，超声波的频率为60-80Hz，振荡时间为40-80min，同时，清洗箱还设置有加热器，加热器为高频感应加热器、内盘管加热器或电极加热器中的一种，且加热器的温度为50-70℃。Preferably, the cleaning liquids in the steps B, F, H and L are all plasma water, and the cleaning methods are ultrasonic vibration cleaning. At the same time, the frequency of the ultrasonic waves is 60-80Hz, and the oscillation time is 40-80min. At the same time, The cleaning box is also provided with a heater, which is one of a high-frequency induction heater, an inner coil heater or an electrode heater, and the temperature of the heater is 50-70°C.
优选的，所述步骤J中的氢氧化物为氢氧化铁、氢氧化亚铁、氢氧化锌、氢氧化镁、氢氧化钴、氢氧化钠、氢氧化钾、氢氧化钡或氢氧化锂中的一种。Preferably, the hydroxide in the step J is ferric hydroxide, ferrous hydroxide, zinc hydroxide, magnesium hydroxide, cobalt hydroxide, sodium hydroxide, potassium hydroxide, barium hydroxide or lithium hydroxide a kind of.
优选的，所述步骤G之前还包括氮气升温：在氮气持续通入的条件下进行程序升温，以10-20℃/min的升温速率，设定在900-1100℃温度区间内煅烧2.5-4h。Preferably, before the step G, it also includes nitrogen heating: program heating under the condition that nitrogen is continuously introduced, and calcining at a temperature range of 900-1100 °C for 2.5-4 h at a heating rate of 10-20 °C/min. .
优选的，所述步骤K中的表面活性剂为氯化十六烷基吡啶、十二烷基硫酸钠、十二烷基苯磺酸钠、吐温或司班中的一种。Preferably, the surfactant in the step K is one of cetyl pyridine chloride, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, Tween or Span.
优选的，所述步骤C、F、I和M中的烘干温度均为100-150℃，且烘干时间均为60-90min。Preferably, the drying temperatures in the steps C, F, I and M are all 100-150° C., and the drying times are all 60-90 min.
优选的，所述步骤J和K中的浸泡温度均为80-100℃，且浸泡时间均为4-6h，同时，间隔30-60min搅拌一次，每次搅拌2-4min。Preferably, the soaking temperatures in the steps J and K are both 80-100° C., and the soaking times are both 4-6 hours. At the same time, stirring is performed once every 30-60 minutes, and each stirring is 2-4 minutes.
有益效果beneficial effect
与现有技术相比，本发明的有益效果如下：本发明将活性炭纤维在镁粉中进行第一次改性，在管式炉中进行高温氨气和氮气进行第二次改性，最后在表面活性剂中浸泡后在氮气、水蒸气和二氧化碳的混合气体中进行第三次改性，可有效提高活性炭纤维的扩孔效果，且对活性炭纤维的整体强度不产生影响，从而扩大了其市场竞争力，符合企业自身的利益。Compared with the prior art, the beneficial effects of the present invention are as follows: in the present invention, activated carbon fibers are modified in magnesium powder for the first time, and high-temperature ammonia and nitrogen are modified for the second time in a tube furnace. After being soaked in surfactant, the third modification is carried out in a mixed gas of nitrogen, water vapor and carbon dioxide, which can effectively improve the pore-enlarging effect of activated carbon fibers, and has no effect on the overall strength of activated carbon fibers, thus expanding its market. Competitiveness is in the interests of the enterprise itself.
本发明的实施方式Embodiments of the present invention
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, but not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
活性炭纤维的扩孔方法，其扩孔方法包括以下步骤：A、除杂：将活性炭纤维送入静电除杂箱内进行表面除杂处理；B、第一次清洗：将除杂后的活性炭纤维送入清洗箱内进行清洗处理；C、第一次烘干：将清洗后的活性炭纤维送入干燥箱内进行干燥处理；D、第一次改性：将干燥后的活性炭纤维置于镁粉中反应30-70min，且反应温度为900-1300℃；E、第二次清洗：将第一次改性后的活性炭纤维送入清洗箱内进行清洗处理；F、第二次烘干：将清洗后的活性炭纤维送入干燥箱内进行干燥处理；G、第二次改性：将干燥后活性炭纤维置于管式炉中进行高温氨气改性，然后将改性后的活性炭纤维置于管式炉中，继续在氮气气氛下以一定的升温速率升温至300℃，然后切换至氨气气氛下，继续升温至900-1100℃，在此温度下进行高温改性，且改性时间2-3h；H、第三次清洗：将第二次改性后的活性炭纤维送入清洗箱内进行清洗处理；I、第三次烘干：将清洗后的活性炭纤维送入干燥箱内进行干燥处理；J、浸泡：将干燥后的活性炭纤维浸泡于乙醇溶液中，并在乙醇溶液中加入氢氧化物为扩孔剂；K、第三次改性：将浸泡后的活性炭纤维继续浸泡在表面活性剂中，并在在氮气保护下加热2-4h，且加热温度为300-500℃，然后将氮气切换成水蒸气和二氧化碳的混合气体，并继续在700-800℃下加热1-3h；L、第四次清洗：将第三次改性后的活性炭纤维送入清洗箱内进行清洗处理；M、第四次烘干：将清洗后的活性炭纤维送入干燥箱内进行干燥处理，得到扩孔活性炭纤维。A method for expanding the pores of activated carbon fibers, which includes the following steps: A. Impurity removal: the activated carbon fibers are sent into an electrostatic trash removal box for surface impurity removal treatment; B. The first cleaning: the activated carbon fibers after removal of impurities are cleaned Send it into a cleaning box for cleaning treatment; C. Drying for the first time: send the cleaned activated carbon fiber into a drying box for drying treatment; D. First modification: place the dried activated carbon fiber on magnesium powder The middle reaction is 30-70min, and the reaction temperature is 900-1300 ℃; E, the second cleaning: the activated carbon fiber after the first modification is sent into the cleaning box for cleaning; F, the second drying: the The cleaned activated carbon fibers are sent to a drying box for drying; G. Second modification: place the dried activated carbon fibers in a tube furnace for high-temperature ammonia modification, and then place the modified activated carbon fibers in a In the tube furnace, continue to heat up to 300°C at a certain heating rate in a nitrogen atmosphere, then switch to an ammonia atmosphere, continue to heat up to 900-1100°C, and perform high-temperature modification at this temperature, and the modification time is 2 -3h; H, cleaning for the third time: the activated carbon fiber after the second modification is sent into the cleaning box for cleaning treatment; 1, drying for the third time: the activated carbon fiber after cleaning is sent into the drying box for drying Treatment; J. Soaking: soak the dried activated carbon fibers in an ethanol solution, and add hydroxide to the ethanol solution as a pore-enlarging agent; K. The third modification: continue to soak the soaked activated carbon fibers on the surface The active agent is heated under nitrogen protection for 2-4h, and the heating temperature is 300-500℃, then the nitrogen is switched to a mixed gas of water vapor and carbon dioxide, and the heating is continued at 700-800℃ for 1-3h; L, the fourth cleaning: the activated carbon fiber after the third modification is sent into the cleaning box for cleaning treatment; M, the fourth drying: the activated carbon fiber after the cleaning is sent into the drying box for drying treatment to obtain Pore-enlarging activated carbon fibers.
将活性炭纤维在镁粉中进行第一次改性，在管式炉中进行高温氨气和氮气进行第二次改性，最后在表面活性剂中浸泡后在氮气、水蒸气和二氧化碳的混合气体中进行第三次改性，可有效提高活性炭纤维的扩孔效果，且对活性炭纤维的整体强度不产生影响，从而扩大了其市场竞争力，符合企业自身的利益。The activated carbon fiber is modified for the first time in magnesium powder, the second modification is carried out with high temperature ammonia and nitrogen in a tube furnace, and finally soaked in a surfactant and then in a mixed gas of nitrogen, water vapor and carbon dioxide. The third modification can effectively improve the pore-enlarging effect of the activated carbon fiber without affecting the overall strength of the activated carbon fiber, thereby expanding its market competitiveness and conforming to the interests of the enterprise itself.
步骤B、F、H和L中的清洗液均为等离子水，且清洗方式均为超声波震荡清洗，同时，超声波的频率为60-80Hz，振荡时间为40-80min，同时，清洗箱还设置有加热器，加热器为高频感应加热器、内盘管加热器或电极加热器中的一种，且加热器的温度为50-70℃。The cleaning solutions in steps B, F, H and L are all plasma water, and the cleaning methods are ultrasonic vibration cleaning. At the same time, the frequency of the ultrasonic wave is 60-80Hz, and the oscillation time is 40-80min. At the same time, the cleaning box is also provided with The heater is one of a high-frequency induction heater, an inner coil heater or an electrode heater, and the temperature of the heater is 50-70°C.
步骤J中的氢氧化物为氢氧化铁、氢氧化亚铁、氢氧化锌、氢氧化镁、氢氧化钴、氢氧化钠、氢氧化钾、氢氧化钡或氢氧化锂中的一种。The hydroxide in step J is one of ferric hydroxide, ferrous hydroxide, zinc hydroxide, magnesium hydroxide, cobalt hydroxide, sodium hydroxide, potassium hydroxide, barium hydroxide or lithium hydroxide.
步骤G之前还包括氮气升温：在氮气持续通入的条件下进行程序升温，以10-20℃/min的升温速率，设定在900-1100℃温度区间内煅烧2.5-4h。Before step G, nitrogen heating is also included: the temperature is programmed under the condition that nitrogen is continuously introduced, and calcination is set at a temperature range of 900-1100 °C for 2.5-4 hours at a heating rate of 10-20 °C/min.
步骤K中的表面活性剂为氯化十六烷基吡啶、十二烷基硫酸钠、十二烷基苯磺酸钠、吐温或司班中的一种。The surfactant in step K is a kind of in cetyl pyridine chloride, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, Tween or span.
步骤C、F、I和M中的烘干温度均为100-150℃，且烘干时间均为60-90min。The drying temperatures in steps C, F, I and M are all 100-150° C., and the drying times are all 60-90 min.
步骤J和K中的浸泡温度均为80-100℃，且浸泡时间均为4-6h，同时，间隔30-60min搅拌一次，每次搅拌2-4min。The soaking temperatures in steps J and K are both 80-100° C., and the soaking times are both 4-6 h. At the same time, stirring is performed once at intervals of 30-60 minutes, and stirring is performed for 2-4 minutes each time.
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, and substitutions can be made in these embodiments without departing from the principle and spirit of the invention and modifications, the scope of the invention is defined by the appended claims and their equivalents.

Claims (7)

  1. 活性炭纤维的扩孔方法，其特征在于：其扩孔方法包括以下步骤：A、除杂：将活性炭纤维送入静电除杂箱内进行表面除杂处理；B、第一次清洗：将除杂后的活性炭纤维送入清洗箱内进行清洗处理；C、第一次烘干：将清洗后的活性炭纤维送入干燥箱内进行干燥处理；D、第一次改性：将干燥后的活性炭纤维置于镁粉中反应30-70min，且反应温度为900-1300℃；E、第二次清洗：将第一次改性后的活性炭纤维送入清洗箱内进行清洗处理；F、第二次烘干：将清洗后的活性炭纤维送入干燥箱内进行干燥处理；G、第二次改性：将干燥后活性炭纤维置于管式炉中进行高温氨气改性，然后将改性后的活性炭纤维置于管式炉中，继续在氮气气氛下以一定的升温速率升温至300℃，然后切换至氨气气氛下，继续升温至900-1100℃，在此温度下进行高温改性，且改性时间2-3h；H、第三次清洗：将第二次改性后的活性炭纤维送入清洗箱内进行清洗处理；I、第三次烘干：将清洗后的活性炭纤维送入干燥箱内进行干燥处理；J、浸泡：将干燥后的活性炭纤维浸泡于乙醇溶液中，并在乙醇溶液中加入氢氧化物为扩孔剂；K、第三次改性：将浸泡后的活性炭纤维继续浸泡在表面活性剂中，并在在氮气保护下加热2-4h，且加热温度为300-500℃，然后将氮气切换成水蒸气和二氧化碳的混合气体，并继续在700-800℃下加热1-3h；L、第四次清洗：将第三次改性后的活性炭纤维送入清洗箱内进行清洗处理；M、第四次烘干：将清洗后的活性炭纤维送入干燥箱内进行干燥处理，得到扩孔活性炭纤维。The hole-enlarging method of activated carbon fiber is characterized in that: the hole-enlarging method includes the following steps: A. Impurity removal: sending the activated carbon fiber into an electrostatic cleaning box for surface cleaning treatment; B. Cleaning for the first time: removing impurities The activated carbon fibers are sent into the cleaning box for cleaning treatment; C. The first drying: the cleaned activated carbon fibers are sent into the drying box for drying treatment; D. The first modification: the dried activated carbon fibers are Placed in magnesium powder and reacted for 30-70min, and the reaction temperature was 900-1300 ℃; E. Second cleaning: The activated carbon fiber after the first modification was sent into the cleaning box for cleaning; F. The second time Drying: send the cleaned activated carbon fibers into a drying box for drying; G. Second modification: place the dried activated carbon fibers in a tube furnace for high-temperature ammonia modification, and then The activated carbon fibers are placed in a tube furnace, continue to heat up to 300°C at a certain heating rate in a nitrogen atmosphere, and then switch to an ammonia atmosphere, continue to heat up to 900-1100°C, and perform high-temperature modification at this temperature, and Modification time 2-3h; H, cleaning for the third time: the activated carbon fiber after the second modification is sent into the cleaning box for cleaning treatment; 1, drying for the third time: the activated carbon fiber after cleaning is sent into drying Dry treatment in the box; J. Soaking: soak the dried activated carbon fibers in an ethanol solution, and add hydroxide to the ethanol solution as a pore-enlarging agent; K. The third modification: soak the activated carbon fibers after soaking Continue to soak in the surfactant and heat for 2-4h under nitrogen protection, and the heating temperature is 300-500℃, then switch the nitrogen gas to the mixed gas of water vapor and carbon dioxide, and continue to heat at 700-800℃ 1-3h; L, the fourth cleaning: send the activated carbon fibers after the third modification into the cleaning box for cleaning; M, the fourth drying: send the cleaned activated carbon fibers into the drying box for cleaning After drying, the pore-enlarging activated carbon fiber is obtained.
  2. 根据权利要求1所述的活性炭纤维的扩孔方法，其特征在于：所述步骤B、F、H和L中的清洗液均为等离子水，且清洗方式均为超声波震荡清洗，同时，超声波的频率为60-80Hz，振荡时间为40-80min，同时，清洗箱还设置有加热器，加热器为高频感应加热器、内盘管加热器或电极加热器中的一种，且加热器的温度为50-70℃。The hole-reaming method of activated carbon fiber according to claim 1, wherein the cleaning solutions in the steps B, F, H and L are all plasma water, and the cleaning methods are ultrasonic vibration cleaning. The frequency is 60-80Hz, and the oscillation time is 40-80min. At the same time, the cleaning box is also provided with a heater. The heater is one of a high-frequency induction heater, an inner coil heater or an electrode heater. The temperature is 50-70°C.
  3. 根据权利要求1所述的活性炭纤维的扩孔方法，其特征在于：所述步骤J中的氢氧化物为氢氧化铁、氢氧化亚铁、氢氧化锌、氢氧化镁、氢氧化钴、氢氧化钠、氢氧化钾、氢氧化钡或氢氧化锂中的一种。The hole-enlarging method of activated carbon fiber according to claim 1, wherein the hydroxide in the step J is ferric hydroxide, ferrous hydroxide, zinc hydroxide, magnesium hydroxide, cobalt hydroxide, hydrogen One of sodium oxide, potassium hydroxide, barium hydroxide or lithium hydroxide.
  4. 根据权利要求1所述的活性炭纤维的扩孔方法，其特征在于：所述步骤G之前还包括氮气升温：在氮气持续通入的条件下进行程序升温，以10-20℃/min的升温速率，设定在900-1100℃温度区间内煅烧2.5-4h。The hole-enlarging method of activated carbon fiber according to claim 1, characterized in that: before the step G, it also includes nitrogen heating: under the condition that nitrogen is continuously introduced, the temperature is programmed at a heating rate of 10-20 °C/min. , set at 900-1100 ℃ temperature range calcination 2.5-4h.
  5. 根据权利要求1所述的活性炭纤维的扩孔方法，其特征在于：所述步骤K中的表面活性剂为氯化十六烷基吡啶、十二烷基硫酸钠、十二烷基苯磺酸钠、吐温或司班中的一种。The hole-enlarging method of activated carbon fiber according to claim 1, wherein the surfactant in the step K is cetyl pyridine chloride, sodium dodecyl sulfate, dodecyl benzene sulfonic acid One of Sodium, Tween or Span.
  6. 根据权利要求1所述的活性炭纤维的扩孔方法，其特征在于：所述步骤C、F、I和M中的烘干温度均为100-150℃，且烘干时间均为60-90min。The hole-enlarging method of activated carbon fiber according to claim 1, characterized in that: the drying temperatures in the steps C, F, I and M are all 100-150° C., and the drying times are all 60-90 min.
  7. 根据权利要求1所述的活性炭纤维的扩孔方法，其特征在于：所述步骤J和K中的浸泡温度均为80-100℃，且浸泡时间均为4-6h，同时，间隔30-60min搅拌一次，每次搅拌2-4min。The method for expanding the pores of activated carbon fibers according to claim 1, wherein the soaking temperature in the steps J and K is 80-100°C, and the soaking time is 4-6h, and at the same time, the interval is 30-60min Stir once, 2-4min each time.
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