CN112941965B - Carbon fiber filter paper and preparation method thereof - Google Patents

Carbon fiber filter paper and preparation method thereof Download PDF

Info

Publication number
CN112941965B
CN112941965B CN202110105504.XA CN202110105504A CN112941965B CN 112941965 B CN112941965 B CN 112941965B CN 202110105504 A CN202110105504 A CN 202110105504A CN 112941965 B CN112941965 B CN 112941965B
Authority
CN
China
Prior art keywords
carbon fiber
fibers
carbon
filter paper
parts
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202110105504.XA
Other languages
Chinese (zh)
Other versions
CN112941965A (en
Inventor
王一苇
贾金升
那天一
孙勇
余刚
孟政
孔壮
杨亮亮
孟凡禹
刘波
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Building Materials Academy CBMA
Original Assignee
China Building Materials Academy CBMA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Building Materials Academy CBMA filed Critical China Building Materials Academy CBMA
Priority to CN202110105504.XA priority Critical patent/CN112941965B/en
Publication of CN112941965A publication Critical patent/CN112941965A/en
Application granted granted Critical
Publication of CN112941965B publication Critical patent/CN112941965B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H27/00Special paper not otherwise provided for, e.g. made by multi-step processes
    • D21H27/08Filter paper
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • B01D39/20Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2055Carbonaceous material
    • B01D39/2065Carbonaceous material the material being fibrous
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/21Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/22Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/02Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
    • D06M13/51Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
    • D06M13/513Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H13/00Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H13/00Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
    • D21H13/36Inorganic fibres or flakes
    • D21H13/46Non-siliceous fibres, e.g. from metal oxides
    • D21H13/50Carbon fibres
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/06Paper forming aids
    • D21H21/08Dispersing agents for fibres
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/06Paper forming aids
    • D21H21/12Defoamers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/06Filter cloth, e.g. knitted, woven non-woven; self-supported material
    • B01D2239/0604Arrangement of the fibres in the filtering material
    • B01D2239/0636Two or more types of fibres present in the filter material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/10Filtering material manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/12Special parameters characterising the filtering material
    • B01D2239/1225Fibre length
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/40Fibres of carbon

Abstract

The invention relates to carbon fiber filter paper and a preparation method thereof. The method comprises the following steps: 1) activating raw material carbon fibers to obtain first carbon fibers; 2) carrying out electrochemical oxidation surface treatment on the first carbon fibers to obtain second carbon fibers; 3) cutting the second carbon fiber, soaking the second carbon fiber by using a first coupling agent, and performing ultrasonic treatment to obtain a third carbon fiber; 4) soaking other fibers by using a second coupling agent and carrying out ultrasonic treatment; 5) adding water to the third carbon fibers and the other fibers treated in the step 4) for defibering, pulping, and papermaking and forming to obtain carbon fiber base paper; 6) and carrying out resin compounding on the carbon fiber base paper to obtain the carbon fiber filter paper. The technical problem to be solved is to ensure that the carbon fiber filter paper has good uniformity, large adsorption capacity and small filtration resistance, thereby being more suitable for practicality.

Description

Carbon fiber filter paper and preparation method thereof
Technical Field
The invention belongs to the technical field of filter material manufacturing, and particularly relates to carbon fiber filter paper and a preparation method thereof.
Background
Various high-performance materials are continuously discovered and applied in the world, wherein carbon fiber becomes one of the most rapidly developed novel materials in recent years by virtue of the characteristics of high temperature resistance, corrosion resistance, small thermal expansion coefficient, good dimensional stability, high strength, high modulus and the like, and is widely applied to processing and preparing novel high-performance composite materials, such as carbon fiber paper. The carbon fiber paper is used for the aspects of filter materials, proton exchange diffusion layer materials of fuel cells, electromagnetic shielding materials, antistatic packaging materials, heating materials and the like by virtue of the characteristics of porosity, excellent heat conduction and electric heating performance, good mechanical performance and the like, and different application fields also put forward different requirements on the performance of the carbon fiber paper.
Carbon fiber paper is generally made by mixing carbon fibers with other fibers. In the production process, the carbon-carbon structures among molecules are mostly connected by nonpolar covalent bonds, the surface active groups are few, the hydrophobicity is easy to appear, the carbon-carbon paper is easy to flocculate in water and difficult to disperse uniformly, in addition, only a cutting effect can be generated in the beating process of the carbon fibers, the phenomenon of devillicate brooming cannot be generated, and hydrogen bonds can not be generated among fibers after paper sheets are formed, so that the uniformity and the strength of the final carbon fiber paper are reduced.
In the prior art, the problem of poor dispersion uniformity of carbon fiber paper is generally solved by adding proper surfactant and dispersant to properly reduce the dispersion concentration of fibers. On one hand, the method adds more surfactant and dispersant, so that the water after papermaking contains a large amount of organic chemical substances, which causes more serious pollution; on the other hand, this method can only solve the problem of poor dispersion uniformity of carbon fiber paper, but cannot improve the adsorption amount and reduce the filtration resistance when it is used as a filter material.
Disclosure of Invention
The invention mainly aims to provide carbon fiber filter paper and a preparation method thereof, and aims to solve the technical problems of good uniformity, large adsorption capacity and small filtration resistance of the carbon fiber filter paper, so that the carbon fiber filter paper is more practical.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. The preparation method of the carbon fiber filter paper provided by the invention comprises the following steps:
1) activating raw material carbon fibers to obtain first carbon fibers;
2) carrying out electrochemical oxidation surface treatment on the first carbon fibers to obtain second carbon fibers;
3) cutting the second carbon fibers, soaking the second carbon fibers in a first coupling agent, and performing ultrasonic treatment to obtain third carbon fibers;
4) soaking other fibers by using a second coupling agent and carrying out ultrasonic treatment;
5) adding water to the third carbon fibers and the other fibers treated in the step 4) for defibering, pulping, and papermaking and forming to obtain carbon fiber base paper;
6) and carrying out resin compounding on the carbon fiber base paper to obtain the carbon fiber filter paper.
The purpose of the invention and the technical problem to be solved can be further realized by adopting the following technical measures.
Preferably, in the above preparation method, the preparation steps of the raw carbon fiber are as follows:
01) soaking and washing PAN precursor fibers by an organic solvent and carrying out ultrasonic treatment for 30-60 min;
02) pre-oxidizing the PAN precursor fiber treated in the step 01); wherein the pre-oxidation treatment adopts gradient temperature rise, the initial temperature is 200-230 ℃, the termination temperature is 250-280 ℃, the pre-oxidation time is 50-90 min, and the atmosphere is air;
03) carbonizing the PAN precursor fiber treated in the step 02) to obtain a raw material carbon fiber; the temperature of the carbonization treatment is 350-750 ℃, the time is 1-5 min, and the atmosphere is nitrogen.
Preferably, in the preparation method, the activation treatment in the step 1) is steam activation, the flow rate of the steam is 0.1-2 g/min, the temperature is 750-1000 ℃, the time is 10-60 min, and the sample collection tension is 400-500N.
Preferably, in the preparation method, the electrochemical oxidation surface treatment in the step 2) is performed by using 0.1 to 1mol/L ammonium bicarbonate as an electrolyte solution, and the current density is 0.1 to 0.3mA/cm 2 The electrolysis temperature is 30 ℃, and the electrolysis time is 60-180 s; washing the second carbon fibers with circulating distilled water.
Preferably, in the preparation method, the length of the third carbon fiber in the step 3) is 2-10 mm; the first coupling agent is at least one selected from the group consisting of KH-550, KH-560, TMc-102 and TMc-6070.
Preferably, the aforementioned production method, wherein the other fiber comprises a plant fiber and a heat-fusible fiber; the plant fiber is selected from at least one of wood fiber, bamboo fiber, hemp fiber and cellulose nanofiber; the second coupling agent is selected from KH-550 or KH-560.
Preferably, in the preparation method, the other fibers comprise plant fibers and hot melt fibers; the raw materials for preparing the carbon fiber filter paper comprise, by mass, 20-50 parts of third carbon fibers, 20-70 parts of plant fibers and 10-40 parts of hot-melt fibers.
Preferably, in the preparation method, during the hydrolysis in the step 5), a defoaming agent, 1-10 parts by mass of a dispersing agent and 5-30 parts by mass of an adhesive are added, the hydrolysis time is 30-120 min, and the rotation speed is 5000-15000 rpm; the mass concentration of the pulp slurry obtained by defibering is 1-3 thousandths; the beating degree of the paper pulp obtained by beating is 20-60 degrees SR.
Preferably, the aforementioned production method, wherein the dispersant is at least one selected from the group consisting of polyethylene oxide, carboxymethyl cellulose, and anionic polyacrylamide; the adhesive is polyvinyl alcohol.
Preferably, in the preparation method, the resin compounding in step 6) includes the following steps:
61) dipping the carbon fiber base paper in a phenolic resin ethanol solution with the mass concentration of 5-20%; the dosage of the phenolic resin is 40-200 parts by mass;
62) adding 20-60 parts by mass of carbon graphite micropowder into the phenolic resin ethanol solution;
63) drying the impregnated carbon fiber base paper at 60-80 ℃ for 30-120 min, applying pressure of 0.1-4.0 Mpa to the surface of the paper at 100-300 ℃ and squeezing for 2-20 min to obtain the carbon fiber filter paper.
Preferably, the above production method, wherein the carbon graphite fine powder is at least one selected from the group consisting of carbon black, graphite powder and expanded graphite; the particle size is 1 to 6 μm.
The object of the present invention and the technical problem to be solved are also achieved by the following technical means. The carbon fiber filter paper prepared according to the method has the air permeability of more than or equal to 60L/s.m 2 The soil-receiving capacity is more than or equal to 100g/m 2 The filtration efficiency is more than or equal to 99 percent, the tensile strength is more than or equal to 1.3kN/m, and the burst strength is more than or equal to 190 kPa.
By means of the technical scheme, the carbon fiber filter paper and the preparation method thereof provided by the invention at least have the following advantages:
1. the PAN-based carbon fiber is subjected to activation treatment, the specific surface area of the PAN-based carbon fiber is increased, the first carbon fiber with a rich pore structure is prepared, a large number of micropores are mainly uniformly distributed on the surface of the first carbon fiber, and the adsorption energy of the PAN-based carbon fiber to organic toxic gas is far stronger than that of common carbon fiber under the air atmosphere condition or in a solution, so that the adsorption capacity of the PAN-based carbon fiber filter paper is improved, and the adsorption and desorption rates of the PAN-based carbon fiber filter paper are effectively and obviously improved;
2. according to the invention, the electrochemical oxidation surface treatment is further carried out on the PAN-based first carbon fiber to prepare the second carbon fiber, so that a large number of oxygen-containing functional groups such as carboxyl, carbonyl, ester, peroxide and the like are formed on the surface of the fiber, the grooves and the surface area of the surface of the fiber are increased, the surface energy and the wettability of the fiber are improved, the hydrophilicity of the second carbon fiber and the dispersibility of the second carbon fiber in water are further improved, and the uniformity of the prepared carbon fiber filter paper is improved; in addition, the dosage of the surfactant and the dispersant can be reduced through the activating treatment and the electrochemical oxidation surface treatment process, so that the organic chemical substances contained in the water after papermaking are reduced, and the environment is protected;
3. according to the invention, the third carbon fiber and one or more of the plant fiber and the hot melt fiber are used as the adhesive fiber, and the preparation method for carrying out mixed papermaking forming on the carbon fiber and the adhesive fiber is adopted, in the prepared filter paper, the active carbon fiber is similar to a steel bar support in a reinforced concrete structure to play a role in the whole structure, and the adhesive fiber is similar to cement to play a role in bonding, so that the synergistic effect of various fibers in the filter paper is ensured to the maximum extent, and the synthesized PAN-based carbon fiber filter paper has certain uniformity and initial strength;
4. according to the invention, the carbon fiber and the bonding fiber are modified by the coupling agent with excellent performance, and the active groups on the surface of the fiber are increased, so that the dispersion effect of the fiber in water is improved; in addition, a plurality of dispersants and adhesives are added in the defibering process to perform a synergistic effect, hydrophilic groups contained in molecular chains of the dispersants reduce the surface tension of PAN-based carbon fibers, and are beneficial to wetting the carbon fibers by water, and the surfaces of the activated carbon fibers can be provided with static electricity, so that the fibers are mutually repelled due to the static electricity, the flocculation of the carbon fibers is prevented, the dispersion effect of the activated carbon fibers in water is further improved, the adhesives are beneficial to the function of serving as binders in the process of manufacturing and forming wet paper pages, the PAN-based activated carbon fibers and the bonding fibers are tightly bonded together, and the enhancement of the performance of the filter paper is facilitated;
5. the PAN-based carbon fiber filter paper prepared by the method has the advantages of large adsorption capacity, small filtration resistance, high dispersion uniformity and high strength, the filtration efficiency is more than or equal to 99%, and the pollutant carrying capacity is more than or equal to 100g/m 2 Air permeability of not less than 60L/s.m 2 Tensile strength of 1.5kN/m or moreThe burst strength is more than or equal to 200 kPa; the comprehensive performance of the composite material is superior to that of products on the market, so that the composite material has wide market prospect and great economic benefit value.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description will be given to specific embodiments, structures, characteristics and effects of the carbon fiber filter paper and the preparation method thereof according to the present invention with reference to the preferred embodiments.
The invention provides a preparation method of carbon fiber filter paper, which comprises the following steps: 1) activating raw material carbon fibers to obtain first carbon fibers; 2) carrying out electrochemical oxidation surface treatment on the first carbon fibers to obtain second carbon fibers; 3) cutting the second carbon fiber, soaking the second carbon fiber by using a first coupling agent, and performing ultrasonic treatment to obtain a third carbon fiber; 4) soaking other fibers by using a second coupling agent and carrying out ultrasonic treatment; 5) the third carbon fiber and other fibers treated in the step 4) are subjected to hydrolysis, papermaking and forming to obtain carbon fiber base paper; 6) and carrying out resin compounding on the carbon fiber base paper to obtain the carbon fiber filter paper.
As the raw material carbon fiber, commercially available carbon fibers can be used.
In order to further stably control the performance of the carbon fiber filter paper, the PAN precursor fiber is preferably used for preparing the raw material carbon fiber by self.
Preferably, the preparation steps of the raw carbon fiber are as follows:
01) soaking and washing PAN precursor fibers by an organic solvent and carrying out ultrasonic treatment for 30-60 min; 02) pre-oxidizing the PAN precursor fiber treated in the step 01); wherein the pre-oxidation treatment adopts gradient temperature rise, the initial temperature is 200-230 ℃, the termination temperature is 250-280 ℃, the pre-oxidation time is 50-90 min, and the atmosphere is air; 03) carbonizing the PAN precursor fiber treated in the step 02) to obtain a raw material carbon fiber; the temperature of the carbonization treatment is 350-750 ℃, the time is 1-5 min, and the atmosphere is nitrogen.
The PAN precursor fiber is Polyacrylonitrile fiber and is named Polyacrylonitile in English.
The organic solvent is subjected to dipping and ultrasonic treatment in the step 01), and the aim of the method is to remove a small amount of impurities on the surface of the PAN precursor fiber so as to improve the purity of the PAN precursor fiber. Wherein, the organic solvent is preferably acetone.
The PAN precursor fiber is converted into the carbon fiber after being subjected to pre-oxidation treatment and carbonization treatment, which is a complex physical and chemical process. In this process, the PAN precursor fibers change from flexible material to brittle material carbon fibers.
The pre-oxidation treatment in the step 02) is carried out in the air. The continuous pre-oxidation furnace is divided into a plurality of temperature zones, the temperature of each temperature zone is set to be a constant value, and the temperature of the furnace zone is increased in a step mode. The fiber runs from the low temperature furnace area to the high temperature furnace area.
Preferably, the number of the temperature zones is 4-10; preferably, the temperature zone comprises 4-6.
Preferably, the initial temperature of the pre-oxidation treatment is 200-215 ℃.
Preferably, the termination temperature of the pre-oxidation treatment is 250-260 ℃, 260-265 ℃, 265-270 ℃ and 270-280 ℃.
Preferably, the activation treatment in the step 1) is steam activation, the flow rate of the steam is 0.1-2 g/min, the temperature is 750-1000 ℃, the time is 10-60 min, and the sample collection tension is 400-500N.
Preferably, the temperature of the activation treatment is 900-1000 ℃, and the time is 40-60 min.
According to the technical scheme, the PAN-based carbon fiber is subjected to activation treatment, the specific surface area of the PAN-based carbon fiber is increased, the activated carbon fiber with a rich pore structure, namely the first carbon fiber, is prepared, a large number of micropores are mainly uniformly dispersed on the surface of the carbon fiber, and the adsorption capacity of the PAN-based carbon fiber to organic toxic gas is far higher than that of the ordinary carbon fiber no matter in air atmosphere or in solution, so that the adsorption capacity of the PAN-based carbon fiber filter paper is improved, and the adsorption and desorption rates of the PAN-based carbon fiber filter paper are obviously improved.
Preferably, the electrochemical oxidation surface treatment in the step 2) is to use 0.1-1 mol/L ammonium bicarbonate as an electrolyte solution, and the current density is 0.1-0.3 mA/cm 2 The electrolysis temperature is 30 ℃, and the electrolysis time is 60-180 s; washing the second carbon fibers with recycled distilled water.
The electrolyte solution is not limited to the above-described ammonium bicarbonate solution, and an ammonium bicarbonate solution is preferable.
Preferably, the concentration of the electrolyte solution is 0.5-0.8 mol/L.
The electrolysis temperature is not limited to 30 deg.C, preferably 30 deg.C.
Preferably, the electrolysis time of the electrochemical oxidation surface treatment is 120-180 s.
According to the technical scheme, the first carbon fiber is subjected to electrochemical oxidation surface treatment, so that a large number of oxygen-containing functional groups such as carboxyl, carbonyl, ester, peroxide and the like are formed on the surface of the first carbon fiber, grooves and surface areas of the surface of the carbon fiber are increased, the surface energy and the wettability of the carbon fiber are improved, the hydrophilicity of the carbon fiber and the dispersibility of the carbon fiber in water are further improved, and the uniformity of the carbon fiber filter paper prepared from the carbon fiber filter paper is improved.
Furthermore, by the process design of activating treatment and electrochemical oxidation surface treatment on the carbon fibers, the dosage of adding a surfactant and a dispersant in the manufacturing process is reduced, so that the amount of organic chemical substances contained in the water after papermaking is greatly reduced, and the environment protection is facilitated.
The second carbon fiber after the electrochemical oxidation surface treatment needs to be cleaned by using circulating distilled water to remove the residual electrolyte on the surface of the fiber.
Preferably, the length of the third carbon fiber in the step 3) is 2-10 mm.
Preferably, the length of the third carbon fiber in the step 3) is 2-5 mm or 5-10 mm.
Preferably, the length of the third carbon fiber of step 3) is 5 mm.
And 3) when the second carbon fibers are cut short, controlling the length of the second carbon fibers to be cut short to 2-10 mm, and then soaking the short fibers with a first coupling agent and carrying out ultrasonic treatment.
Preferably, the first coupling agent is selected from at least one of KH-550, KH-560, TMc-102, and TMc-6070.
Preferably, the first coupling agent is KH-550.
Preferably, the other fibers comprise plant fibers; the plant fiber is at least one selected from wood fiber, bamboo fiber, hemp fiber and cellulose nanofiber.
Preferably, the second coupling agent is selected from KH-550 or KH-560.
Preferably, the second coupling agent is KH-550.
According to the technical scheme, the coupling agent with excellent performance is selected to modify the carbon fibers and the bonding fibers, and active groups on the surfaces of the carbon fibers are increased, so that the dispersion effect of the fibers in water is improved.
Preferably, the other fibers include plant fibers and hot melt fibers; the raw materials for preparing the carbon fiber filter paper comprise, by mass, 20-50 parts of third carbon fibers, 20-70 parts of plant fibers and 10-40 parts of hot-melt fibers.
Preferably, the raw materials for preparing the carbon fiber filter paper comprise, by mass, 20-40 parts of third carbon fibers, 50-70 parts of plant fibers and 10-40 parts of hot-melt fibers.
Preferably, the raw materials for preparing the carbon fiber filter paper comprise, by mass, 40 parts of third carbon fibers, 50 parts of plant fibers and 40 parts of hot-melt fibers.
The total mass parts of the third carbon fibers, the plant fibers and the hot-melt fibers are not limited, and the three fibers can be randomly matched and produced within the preferable range.
Preferably, the step 5) of adding water for defibering further comprises adding a defoaming agent, 1-10 parts by mass of a dispersing agent and 5-30 parts by mass of an adhesive, wherein the defibering time is 30-120 min, and the rotating speed is 5000-15000 rpm; the mass concentration of the pulp slurry obtained by defibering is 1-3 per mill.
Preferably, the step 5) further comprises adding 5-8 parts by mass of a dispersing agent and 15-25 parts by mass of an adhesive; the mass concentration of the pulp slurry obtained by defibering is 1 per mill.
Preferably, the step 5) further comprises adding 5-8 parts by mass of a dispersing agent and 20-25 parts by mass of an adhesive.
Preferably, the step 5) further comprises adding 8 parts by mass of a dispersing agent and 25 parts by mass of an adhesive.
Preferably, the beating degree of the paper pulp obtained by beating in the step 5) is 20-60 DEG SR.
Pulping refers to the physical treatment of fibers suspended in water to give them the characteristics required for paper machine production. The beating degree is an index for measuring the difficulty degree (drainage performance) of the slurry dehydration, and can comprehensively reflect the degrees of fiber cutting, swelling, fibrillation, devillication, fibrillation and the like.
The freeness was measured using a shore freeness tester.
According to the technical scheme, the third carbon fiber and other fibers are subjected to defibering, pulping, papermaking and forming in the subsequent treatment, and a plurality of dispersing agents and adhesives are added in the defibering process for synergistic action, so that the comprehensive performance of the carbon fiber filter paper prepared from the third carbon fiber and other fibers is further improved.
Further, according to the technical scheme, a specific process is designed to prepare carbon fibers from PAN precursor fibers, the carbon fibers are subjected to activation treatment to obtain first carbon fibers, the first carbon fibers are subjected to electrochemical oxidation surface treatment to obtain second carbon fibers, and then the second carbon fibers are cut short, soaked by a coupling agent and subjected to ultrasonic treatment to prepare third carbon fibers; and the third carbon fiber and the bonding fiber are subjected to mixed papermaking forming by using plant fiber and/or hot melt fiber as the bonding fiber, in the carbon fiber filter paper, the carbon fiber supports the whole structure similar to a steel bar in a reinforced concrete structure, and the bonding fiber performs a bonding function similar to cement, so that the synergistic effect of various fibers in the filter paper is ensured to the maximum extent, and the carbon fiber filter paper prepared by the method has good uniformity and initial strength.
Preferably, the dispersant is selected from at least one of polyethylene oxide, carboxymethyl cellulose and anionic polyacrylamide; the adhesive is polyvinyl alcohol.
The addition amount of the defoaming agent is based on defoaming, and 2-3 drops are generally added.
The polyethylene oxide is abbreviated as PEO; carboxymethyl cellulose is abbreviated CMC; the anionic polyacrylamide is abbreviated as APAM; the polyvinyl alcohol is abbreviated PVA.
In the technical scheme, a plurality of dispersants and adhesives are added in the defibering process to perform a synergistic effect; the hydrophilic groups contained in the molecular chain of the dispersing agent reduce the surface tension of the PAN-based activated carbon fiber, are beneficial to wetting the carbon fiber by water, and can enable the surface of the activated carbon fiber to be charged with static electricity, so that the fibers are mutually repelled due to the electrostatic action, the flocculation of the carbon fiber is prevented, and the dispersing effect of the activated carbon fiber in water is further improved; the adhesive plays a role of a binder in the process of manufacturing and forming the wet paper sheet, and is beneficial to tightly binding the active carbon fibers and the binding fibers of the PAN group together, thereby being beneficial to enhancing the performance of the filter paper.
Preferably, the resin compounding of step 6) comprises the following steps: 61) dipping the carbon fiber base paper in a phenolic resin ethanol solution with the mass concentration of 5-20%; the dosage of the phenolic resin is 40-200 parts by mass; 62) adding 20-60 parts by mass of carbon graphite micropowder into the phenolic resin ethanol solution; 63) drying the impregnated carbon fiber base paper at 60-80 ℃ for 30-120 min, applying pressure of 0.1-4.0 Mpa to the surface of the paper at 100-300 ℃ and squeezing for 2-20 min to obtain the carbon fiber filter paper.
Preferably, the using amount of the phenolic resin is 100-200 parts by mass; more preferably 120 to 200 parts, and still more preferably 200 parts.
Preferably, the amount of the carbon graphite micro powder is 30-50 parts by mass; more preferably 40 to 50 parts, and still more preferably 50 parts.
Preferably, the carbon graphite micro powder is selected from at least one of carbon black, graphite powder and expanded graphite; carbon black is more preferred.
Preferably, the particle size of the carbon graphite micro powder is 2 +/-1 mu m.
The invention also provides the carbon fiber filter paper prepared by the method, and the air permeability of the carbon fiber filter paper is more than or equal to 60L/s.m 2 The soil-receiving capacity is more than or equal to 100g/m 2 The filtration efficiency is more than or equal to 99 percent, the tensile strength is more than or equal to 1.3kN/m, and the burst strength is more than or equal to 190 kPa.
Preferably, the tensile strength is 1.5kN/m or more and the burst strength is 215kPa or more, as in examples 1 and 3.
Preferably, the tensile strength is 1.7kN/m or more and the burst strength is 225kPa or more, as in example 3.
The technical solution of the present invention will be further described with reference to the following more specific examples, which should not be construed as limiting the invention thereto. If not stated, the raw materials are purchased from the market; the detection method of the performance index of the paper prepared in the example is as follows:
filtration efficiency, dirt holding capacity: measured according to the method specified in GJB 3820-99.
Air permeability: measured according to the method specified in GB/T5453-1997.
Tensile strength: the measurement was carried out according to the method defined in GB/T453-2002.
Burst strength: measured according to the method specified in GB/T454-2002.
Example 1
1) Preparation of carbon fibers
Soaking and washing PAN protofilament fibers with acetone, and carrying out ultrasonic treatment for 60min to remove a small amount of impurities on the surfaces of the protofilament fibers; carrying out thermal stabilization and pre-oxidation treatment on the impurity-removed PAN precursor fiber in a pre-oxidation furnace, wherein the atmosphere is air, the initial speed of filament running is 20m/h, a gradual heating method is adopted, the pre-oxidation furnace is divided into 4 temperature zones, the temperatures from a first temperature zone to a fourth temperature zone are 215 ℃, 235 ℃, 250 ℃ and 260 ℃, the drafting multiplying power is 1.05 times, and the total time of the pre-oxidation treatment is 60 minutes; and (3) putting the pre-oxidized PAN precursor fiber into a high-carbon furnace in a high-purity nitrogen atmosphere for carbonization treatment, wherein the oxygen content in nitrogen is lower than 1ppm, the temperature is 700 ℃, the retention time is 5 minutes, and the drafting multiplying power is 1.05 times, so that the carbon fiber is obtained.
2) Carbon fiber activation treatment and electrochemical oxidation surface treatment to obtain third carbon fiber
Activating the carbon fiber obtained in the step in a steam activation furnace, wherein the flow rate of steam is 2g/min, the temperature is 900 ℃, the time is 40min, and the sample collection tension is 500N to obtain a first carbon fiber; placing the first carbon fiber into an electrolytic bath for electrochemical oxidation surface treatment, wherein the electrolyte solution is 0.5mol/L ammonium bicarbonate, and the current density is 0.3mA/cm 2 Electrolyzing at 30 ℃ for 120s to obtain second carbon fibers; washing the second carbon fiber with circulating distilled water to remove the residual electrolyte on the surface of the fiber; and (3) chopping the second carbon fibers to 5mm in length, then soaking the second carbon fibers in a KH-550 first coupling agent, wherein the mass fraction of the KH-550 solution is 10%, and performing ultrasonic treatment for 60min to obtain third carbon fibers.
3) Paper pulp preparation
Soaking 70 parts of wood fiber and 10 parts of hot-melt fiber together by mass in a KH-550 second coupling agent, wherein the mass fraction of KH-550 solution is 10%; then, ultrasonic treatment was performed for 60 min. Placing the treated wood fibers, the hot-melt fibers and 20 parts of third carbon fibers into a beating machine together, adding water, defibering and beating, simultaneously adding 5 parts by mass of dispersant Anionic Polyacrylamide (APAM), 20 parts by mass of adhesive polyvinyl alcohol (PVA) and 2-3 drops of defoaming agent into a defibering machine together, and defibering together with the fibers to obtain paper pulp with the pulp concentration of 1 per mill; the stirring speed during the fluffing is 10000rpm, and the fluffing time is 30 min.
4) Preparation of PAN-based carbon fiber filter paper
Making and molding the paper pulp by using a Kaiser method automatic paper making system to prepare PAN-based carbon fiber base paper; the base paper is soaked in a phenolic resin ethanol solution with the concentration of 5%, the resin dosage is 120 parts by mass, carbon black powder with the particle size of about 2 mu m is added, the addition is 40 parts by mass, then the drying is carried out for 60min at the temperature of 80 ℃, the pressing and heating are carried out for 15min at the temperature of 200 ℃, and the surface pressure is 3.0MPa, so that the PAN-based carbon fiber filter paper is obtained.
Through detection, the properties of the carbon fiber filter paper prepared in the embodiment are as follows: filtration99.2% of efficiency and 102.3g/m of pollutant holding capacity 2 Air permeability of 63.4L/s.m 2 Tensile strength 1.54kN/m, and burst strength 216 kPa.
Example 2
1) Carbon fibers were prepared as in example 1.
2) The process steps of the carbon fiber activation treatment and the electrochemical oxidation surface treatment are the same as in example 1. The technological parameters are as follows: the flow rate of the water vapor is 2g/min, the temperature is 1000 ℃, the time is 60min, and the sample collection tension is 500N; 0.8mol/L ammonium bicarbonate as electrolyte solution, and 0.3mA/cm current density 2 The electrolysis temperature is 30 ℃, and the electrolysis time is 180 s.
3) The procedure for the pulp formulation was the same as in example 1. The technological parameters are as follows: 20 parts of plant fiber, 10 parts of hot-melt fiber and 50 parts of third carbon fiber; 5 parts of dispersing agent, 15 parts of adhesive and 2-3 drops of defoaming agent to obtain paper pulp with the pulp concentration of 1 per mill.
4) The process steps for making the PAN-based carbon fiber filter paper are the same as in example 1. The amount of the resin was adjusted to 100 parts by mass and 30 parts by mass of carbon black.
Through detection, the carbon fiber filter paper prepared in the embodiment has the following properties: the filtration efficiency is 99.5 percent, and the pollutant holding capacity is 112.3g/m 2 Air permeability of 60.2L/s.m 2 Tensile strength 1.39kN/m, burst strength 193 kPa.
Example 3
1) Carbon fibers were prepared as in example 1. The process parameters are adjusted as follows: the pre-oxidation furnace is divided into 6 temperature zones, and the temperatures from the first temperature zone to the sixth temperature zone are respectively 200 ℃, 220 ℃, 243 ℃, 255 ℃, 265 ℃ and 270 ℃; the temperature of the carbonization treatment is 750 ℃.
2) The process steps of the carbon fiber activation treatment and the electrochemical oxidation surface treatment are the same as in example 1. The technological parameters are as follows: the flow rate of the water vapor is 2g/min, the temperature is 1000 ℃, the time is 60min, and the sample collection tension is 500N; 0.8mol/L ammonium bicarbonate as electrolyte solution, and 0.3mA/cm current density 2 The electrolysis temperature is 30 ℃, and the electrolysis time is 180 s.
3) The procedure for the pulp formulation was the same as in example 1. The technological parameters are as follows: 50 parts of plant fiber, 40 parts of hot-melt fiber and 40 parts of third carbon fiber; 8 parts of dispersing agent, 25 parts of adhesive and 2-3 drops of defoaming agent to obtain paper pulp with the pulp concentration of 1 per mill.
4) The process steps for making the PAN-based carbon fiber filter paper are the same as in example 1. The amount of the resin was adjusted to 200 parts by mass and the amount of the carbon black was adjusted to 50 parts by mass.
Through detection, the carbon fiber filter paper prepared in the embodiment has the following properties: the filtration efficiency is 99.3 percent, the dirt holding capacity is 107.2g/m2, the air permeability is 63.9L/s.m 2, the tensile strength is 1.75kN/m, and the burst strength is 227 kPa.
Comparative example 1
In the same manner as in example 1, the step of carbon fiber activation treatment was omitted. Through detection, the carbon fiber filter paper prepared by the comparative example has the following properties: the filtration efficiency is 97.2 percent, and the pollutant holding capacity is 83.2g/m 2 Air permeability of 60.9L/s.m 2 Tensile strength 1.59kN/m, and burst strength 225 kPa.
Comparative example 2
In the same manner as in example 1, the step of the electrochemical oxidation surface treatment of carbon fiber was omitted. Through detection, the carbon fiber filter paper prepared by the comparative example has the following properties: the filtration efficiency is 98.8 percent, and the pollutant holding capacity is 99.2g/m 2 Air permeability of 61.7L/s.m 2 Tensile strength 1.23kN/m, burst strength 186 kPa.
Comparative example 3
The same as example 1, the step of carbon fiber activation treatment and the step of carbon fiber electrochemical oxidation surface treatment. Through detection, the carbon fiber filter paper prepared by the comparative example has the following properties: the filtration efficiency is 96.8 percent, and the pollutant holding capacity is 81.0g/m 2 Air permeability of 60.3L/s.m 2 Tensile strength 1.24kN/m, bursting strength 191 kPa.
As can be seen from the performance test results of the carbon fiber filter papers prepared in the above examples 1 to 3, the tensile strength is more than or equal to 1.3kN/m, and the burst strength is more than or equal to 193 kPa; the tensile strength and burst resistance of the filter paper are used to characterize its uniformity; the higher the tensile strength and the higher the bursting strength of the filter paper, the better the mechanical properties, which indicates the better the uniformity of the filter paper, and the results of the performance test of the carbon fiber filter paper prepared in the above examples 1 to 3 show that the air permeability is not less than 60L/s.m 2 Nano, naThe dirt-removing power is more than or equal to 102g/m 2 The filtration efficiency is more than or equal to 99 percent; the air permeability, the dirt holding capacity and the filtering efficiency of the filter paper are used for representing the filtering performance of the filter paper; the higher the air permeability of the filter paper is, the smaller the filtration resistance is, and the better the filtration performance is; the higher the dirt-receiving capacity of the filter paper is, the larger the adsorption capacity of the surface of the filter paper is, and the better the filtering performance is; the higher the filtration efficiency of the filter paper, the better the filtration performance.
As can be seen from the performance test results of the carbon fiber filter papers prepared in the above example 1 and comparative examples 1 to 3, the filtration efficiency, the dirt receiving capacity, and the air permeability of the filter paper can be improved by activating the carbon fibers, which indicates that the activated carbon fibers can improve the filtration performance of the filtration; the tensile strength and the bursting strength of the filter paper are slightly reduced by activating the carbon fibers; by carrying out electrochemical oxidation surface treatment on the carbon fibers, the filtering efficiency, the dirt-holding capacity, the air permeability, the tensile strength and the burst strength of the filter paper can be improved; in particular, the electrochemical oxidation surface treatment of the carbon fiber is particularly obvious for improving the tensile strength and the bursting strength of the filter paper.
Furthermore, the carbon fiber is subjected to activation treatment, so that the pollutant carrying capacity of the filter paper is improved by 22.47%, the carbon fiber is subjected to electrochemical oxidation surface treatment, so that the pollutant carrying capacity of the filter paper is improved by 2.72%, and the carbon fiber is subjected to activation treatment and electrochemical oxidation surface treatment in sequence, so that the pollutant carrying capacity of the filter paper is improved by 26.30%; the air permeability of the filter paper is improved by 2.32% by activating the carbon fibers, the dirt-receiving capacity of the filter paper is improved by 1.00% by performing electrochemical oxidation surface treatment on the carbon fibers, and the dirt-receiving capacity of the filter paper is improved by 5.14% by sequentially performing activating treatment and electrochemical oxidation surface treatment on the carbon fibers.
The features of the invention claimed and/or described in the specification may be combined, and are not limited to the combinations set forth in the claims by the recitations therein. The technical solutions obtained by combining the technical features in the claims and/or the specification also belong to the scope of the present invention.

Claims (11)

1. The preparation method of the carbon fiber filter paper is characterized by comprising the following steps of:
1) activating raw carbon fibers to obtain first carbon fibers; the activation treatment is water vapor activation, the flow rate of water vapor is 0.1-2 g/min, the temperature is 750-1000 ℃, the time is 10-60 min, and the sample collection tension is 400-500N;
2) carrying out electrochemical oxidation surface treatment on the first carbon fibers to obtain second carbon fibers; the electrochemical oxidation surface treatment takes 0.1 to 1mol/L ammonium bicarbonate as electrolyte solution, and the current density is 0.1 to 0.3mA/cm 2 The electrolysis temperature is 30 ℃, and the electrolysis time is 60-180 s;
3) cutting the second carbon fibers, soaking the second carbon fibers in a first coupling agent, and performing ultrasonic treatment to obtain third carbon fibers;
4) soaking other fibers by using a second coupling agent and carrying out ultrasonic treatment; the other fibers comprise plant fibers and hot melt fibers;
5) adding water to the third carbon fiber and other fibers treated in the step 4), defibering, pulping, and papermaking to obtain carbon fiber base paper;
6) and carrying out resin compounding on the carbon fiber base paper to obtain the carbon fiber filter paper.
2. The method according to claim 1, wherein the raw carbon fiber is prepared by the steps of:
01) soaking and washing PAN precursor fibers by an organic solvent and carrying out ultrasonic treatment for 30-60 min;
02) pre-oxidizing the PAN precursor fiber treated in the step 01); wherein the pre-oxidation treatment adopts gradient temperature rise, the initial temperature is 200-230 ℃, the termination temperature is 250-280 ℃, the pre-oxidation time is 50-90 min, and the atmosphere is air;
03) carbonizing the PAN precursor fiber treated in the step 02) to obtain a raw material carbon fiber; the temperature of the carbonization treatment is 350-750 ℃, the time is 1-5 min, and the atmosphere is nitrogen.
3. The method of claim 1, wherein the electrochemical oxidation surface treatment of step 2) further comprises washing the second carbon fibers with recycled distilled water.
4. The production method according to claim 1, wherein the length of the third carbon fiber of step 3) is 2 to 10 mm; the first coupling agent is at least one selected from the group consisting of KH-550, KH-560, TMc-102 and TMc-6070.
5. The method of claim 1, wherein the other fibers include plant fibers and hot melt fibers; the plant fiber is selected from at least one of wood fiber, bamboo fiber, hemp fiber and cellulose nanofiber; the second coupling agent is selected from KH-550 or KH-560.
6. The production method according to claim 1, wherein the raw materials for producing the carbon fiber filter paper comprise, by mass, 20 to 50 parts of third carbon fibers, 20 to 70 parts of plant fibers, and 10 to 40 parts of hot-melt fibers.
7. The preparation method of claim 6, wherein the step 5) of adding water for defibering further comprises adding a defoaming agent, 1-10 parts by mass of a dispersing agent and 5-30 parts by mass of an adhesive, wherein the defibering time is 30-120 min, and the rotation speed is 5000-15000 rpm; the mass concentration of the pulp slurry obtained by defibering is 1-3 thousandths; the beating degree of the paper pulp obtained by beating is 20-60 DEG SR.
8. The production method according to claim 7, characterized in that the dispersant is selected from at least one of polyethylene oxide, carboxymethyl cellulose, and anionic polyacrylamide; the adhesive is polyvinyl alcohol.
9. The method according to claim 7, wherein the resin compounding of step 6) comprises the steps of:
61) dipping the carbon fiber base paper in a phenolic resin ethanol solution with the mass concentration of 5-20%; the dosage of the phenolic resin is 40-200 parts by mass;
62) adding 20-60 parts by mass of carbon graphite micro powder into the phenolic resin ethanol solution;
63) drying the impregnated carbon fiber base paper at 60-80 ℃ for 30-120 min, and applying pressure of 0.1-4.0 Mpa to the surface of the paper at 100-300 ℃ to squeeze the paper for 2-20 min to obtain the carbon fiber filter paper.
10. The production method according to claim 9, wherein the fine carbon graphite powder is at least one selected from the group consisting of carbon black, graphite powder, and expanded graphite; the particle size is 1 to 6 μm.
11. A carbon fiber filter paper prepared according to the method of any one of claims 1 to 10, characterized in that it has an air permeability of 60L/s-m or more 2 The soil-receiving capacity is more than or equal to 100g/m 2 The filtration efficiency is more than or equal to 99 percent, the tensile strength is more than or equal to 1.3kN/m, and the burst strength is more than or equal to 190 kPa.
CN202110105504.XA 2021-01-26 2021-01-26 Carbon fiber filter paper and preparation method thereof Active CN112941965B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110105504.XA CN112941965B (en) 2021-01-26 2021-01-26 Carbon fiber filter paper and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110105504.XA CN112941965B (en) 2021-01-26 2021-01-26 Carbon fiber filter paper and preparation method thereof

Publications (2)

Publication Number Publication Date
CN112941965A CN112941965A (en) 2021-06-11
CN112941965B true CN112941965B (en) 2022-09-27

Family

ID=76237209

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110105504.XA Active CN112941965B (en) 2021-01-26 2021-01-26 Carbon fiber filter paper and preparation method thereof

Country Status (1)

Country Link
CN (1) CN112941965B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113529494B (en) * 2021-07-27 2023-05-02 浙江省林业科学研究院 Preparation method of bamboo-based hybrid fiber felt for VARTM (vacuum forming) composite material
CN113699824B (en) * 2021-08-25 2022-11-11 上海骏珲新材料科技有限公司 Carbon fiber composite conductive paper and preparation method thereof
CN115262277B (en) * 2022-08-01 2023-04-14 浙江科技学院 Alkali lignin subcritical water treatment modified carbon fiber and method and application thereof

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101591868B (en) * 2009-06-23 2011-04-27 东华大学 Preparation for carbon fiber paper used for gas diffusion layer of proton exchange membrane fuel cell
CN105274896A (en) * 2015-11-09 2016-01-27 中国林业科学研究院林产化学工业研究所 Preparation method and evenness measurement method for carbon fiber synthetic paper
CN106436274A (en) * 2016-09-14 2017-02-22 郑州峰泰纳米材料有限公司 Method for treating carbon fiber anodic oxidation surfaces
CN107460777A (en) * 2017-07-31 2017-12-12 华南理工大学 A kind of preparation method of full carbon fibre composite paper
CN111286816B (en) * 2018-12-10 2022-11-29 天津工业大学 Preparation method of polyacrylonitrile-based carbon fiber with smooth surface

Also Published As

Publication number Publication date
CN112941965A (en) 2021-06-11

Similar Documents

Publication Publication Date Title
CN112941965B (en) Carbon fiber filter paper and preparation method thereof
CN110528314A (en) A kind of composite sheet and its preparation method and application of the polyphenylene sulfide superfine fiber containing melt-blown
CN111900418B (en) Preparation method of carbon paper precursor for gas diffusion layer of fuel cell
CN104157815B (en) A kind of Bacterial cellulose porous membrane and preparation method thereof
US11876232B2 (en) Gas diffusion layer for proton exchange membrane fuel cell and preparation method thereof
CA2767204C (en) Porous electrode substrate and method for producing the same
CN113322713B (en) Preparation method of carbon paper with gradient pore structure
CN105870383B (en) A kind of battery capacitor barrier film and preparation method thereof
CN111576079B (en) Conductive carbon paper and preparation method thereof
CN104695040A (en) Preparation method of high-strength polyacrylonitrile nano-composite fiber
JP2009283259A (en) Porous carbon electrode base material
CN115387148A (en) High-conductivity and high-air-permeability gradient-structure carbon fiber paper and preparation method thereof
CN107983303A (en) A kind of preparation method of organic wastewater absorption degradation modified carbon fiber
JP2007080742A (en) Carbon fiber sheet for solid polymer electrolyte fuel cell and its manufacturing method
JP2015193941A (en) sheet-like carbon material
CN109411769A (en) A kind of preparation method of fuel cell long-life carbon fiber paper
KR101425305B1 (en) Manufacturing method of carbon fiber paper using PAN fibrid
CN114709560A (en) Lithium ion battery diaphragm paper and preparation method thereof
JP3442061B2 (en) Flat carbon fiber spun yarn woven structural material
JP5398687B2 (en) Solid electrolyte membrane reinforcement
CN111945460A (en) Method for dispersing short carbon fibers and application
JP5394469B2 (en) Porous electrode substrate manufacturing method and porous electrode substrate
CN107217523B (en) A kind of preparation method of the novel hybride fiber carbon paper for supercapacitor
CN111106292A (en) Hydrophilic heat-resistant lithium ion battery diaphragm and preparation method thereof
CN113846512B (en) Self-supporting activated carbon fiber paper and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant