CN111593478A - Asphalt-based general-grade carbon fiber needled felt and preparation method and application thereof - Google Patents
Asphalt-based general-grade carbon fiber needled felt and preparation method and application thereof Download PDFInfo
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- CN111593478A CN111593478A CN202010496122.XA CN202010496122A CN111593478A CN 111593478 A CN111593478 A CN 111593478A CN 202010496122 A CN202010496122 A CN 202010496122A CN 111593478 A CN111593478 A CN 111593478A
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4209—Inorganic fibres
- D04H1/4242—Carbon fibres
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
- D01F9/15—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues from coal pitch
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/44—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
- D04H1/46—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
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- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Fibers (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention discloses a preparation method of a pitch-based universal carbon fiber needled felt, which comprises the following steps of 1) preparing pitch-based universal carbon fiber filaments for later use; 2) feeding the pitch-based general-grade carbon fiber filament prepared in the step 1) into an opener through a feeding roller to prepare a first-grade pitch-based general-grade carbon fiber short filament; 3) conveying the primary pitch-based universal carbon fiber short filaments prepared in the step 2) into a cotton box by wind, and preparing secondary pitch-based universal carbon fiber short filaments under the action of a conveying nail curtain; 4) conveying the second-stage pitch-based general-grade carbon fiber short filaments prepared in the step 3) into a cotton dropping box, uniformly paving the second-stage pitch-based general-grade carbon fiber short filaments on a cotton conveying curtain, then placing the cotton conveying curtain on a net forming box, uniformly paving the cotton conveying curtain on a net forming curtain, and preparing a pre-punched felt under the action of a pre-punching machine; 5) and (3) carrying out multistage needling treatment on the pre-punched felt prepared in the step (4), and then carrying out edge cutting and rolling. The product prepared by the invention has wide application.
Description
Technical Field
The invention belongs to the technical field of non-woven fabric preparation, and particularly relates to a preparation method of an asphalt-based general-grade carbon fiber needled felt, the prepared asphalt-based general-grade carbon fiber needled felt, and application of the asphalt-based general-grade carbon fiber needled felt.
Technical Field
Currently, the center of gravity of the global composite material is shifting from developed countries in europe and america to asia, the high-speed growth of the asian composite material yield is one of the most obvious trends in the development of the industry, and the world carbon fiber demand will increase at a rate of about 13% every year, with a good prospect. In the twenty-first century, the carbon fiber is widely demanded in various industries and markets, and the demand is huge.
Disclosure of Invention
Researches show that the heat-preservation needled felt with the use temperature of domestic equipment over 2000 ℃ is mainly prepared from polyacrylonitrile and viscose base serving as raw materials. Compared with the pitch-based general-grade carbon fiber needled felt, the carbon fiber needled felt prepared from polyacrylonitrile has poor heat insulation performance, and in the production of photovoltaic crystalline silicon and semiconductor chip crystalline silicon, the heat insulation material made of the pitch-based general-grade carbon fiber needled felt is 10% energy-saving compared with the heat insulation material made of the carbon fiber needled felt prepared from polyacrylonitrile. The viscose-based carbon fiber needled felt has high cost and low yield, and is not suitable for being used as a heat insulation material for high-temperature equipment at the temperature of more than 2000 ℃.
The invention aims to provide a preparation method of an asphalt-based general-grade carbon fiber needled felt and the asphalt-based general-grade carbon fiber needled felt prepared by the method.
The carbon fiber has high strength, high modulus, excellent thermal property, excellent oxidation resistance and the like, and is widely applied to the fields of aerospace, transportation and the like. The carbon fiber preform (needle felt) is a preformed part which is formed by laying carbon fibers into a three-dimensional structure by adopting a non-woven process method, and is a framework of composite materials such as carbon/carbon composite materials, carbon/ceramic composite materials and the like.
The specific scheme is as follows:
a preparation method of a pitch-based universal-grade carbon fiber needled felt comprises the following steps:
1) preparation of the starting materials
Preparing asphalt-based general-grade carbon fiber filaments for later use;
2) opening in one step
Feeding the pitch-based general-grade carbon fiber filament prepared in the step 1) into an opener through a feeding roller to prepare a first-grade pitch-based general-grade carbon fiber short filament;
3) secondary opening
Conveying the primary pitch-based universal carbon fiber short filaments prepared in the step 2) into a cotton box by wind, and preparing secondary pitch-based universal carbon fiber short filaments under the action of a conveying nail curtain;
4) pre-needled felt preparation
Conveying the second-stage pitch-based general-grade carbon fiber short filaments prepared in the step 3) into a cotton dropping box, uniformly paving the second-stage pitch-based general-grade carbon fiber short filaments on a cotton conveying curtain, then placing the cotton conveying curtain on a net forming box, uniformly paving the cotton conveying curtain on a net forming curtain, and preparing a pre-punched felt under the action of a pre-punching machine;
5) needling treatment
And (3) carrying out multistage needling treatment on the pre-punched felt prepared in the step (4), and then carrying out edge cutting and rolling.
In a specific embodiment of the present invention, 1) the method for preparing the pitch-based general-purpose carbon fiber filament in the preparation of raw materials comprises the following steps:
firstly, heating the spun asphalt to the temperature of 280 ℃ and 350 ℃, pressurizing to 1-2.5Mpa by a melt pump, and preparing asphalt protofilaments by a spinning die head;
secondly, the pitch protofilament is oxidized in a pre-oxidation furnace at the temperature of 150 ℃ and 450 ℃ to obtain pre-oxidized fiber;
thirdly, the pre-oxidized fiber is sent into a carbonization furnace, and the pre-oxidized fiber is prepared into the pitch-based universal carbon fiber precursor at the temperature of over 900 ℃ in the nitrogen atmosphere.
In a specific embodiment of the invention, the diameter of the asphalt-based universal carbon fiber precursor is 5-15 μm, the carbon content is more than or equal to 93%, and the true density is 1.4-2.3g/cm3。
In a specific embodiment of the invention, in 2) one-time opening, the length of the first-grade asphalt-based general-grade carbon fiber short filament is 8-12 cm.
In a specific embodiment of the invention, in 3) the secondary opening, the length of the second-level pitch-based general-purpose carbon fiber short filament is 4-5 cm.
In a specific embodiment of the invention, the rotating speed of the opener is 700-; the length of the nails on the nail roller is more than or equal to 25mm, and the nail density of the nail roller is 0.2-0.3 per square centimeter.
In a specific embodiment of the invention, 4) in the preparation of the pre-punched felt, the pre-punched felt is uniformly laid on the thickness of the cotton conveying curtainThe degree is 6-8 cm; the laying gram weight is 500-1000g/m2。
The invention provides an asphalt-based general-grade carbon fiber needled felt which is prepared by any preparation method of the asphalt-based general-grade carbon fiber needled felt.
The invention provides application of an asphalt-based universal carbon fiber needled felt as a heat preservation article in the process of producing and preparing crystalline silicon products.
In a specific embodiment of the invention, the crystalline silicon product comprises photovoltaic crystalline silicon and semiconductor chip crystalline silicon.
Compared with the prior art, the invention has the beneficial effects that:
the molecular structure of the product prepared by the invention is a microscopically ordered, macroscopically disordered isotropic structure, and is not easy to graphitize, and the non-graphitized disordered structure is an ideal structure for heat preservation and heat insulation/radiation blocking. The product prepared by the invention has the characteristics of acid and alkali resistance, high temperature resistance, no combustion, oxidation resistance, sound insulation and the like, is suitable for being used under the high-temperature heat insulation condition, and has wide application.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Example 1
A preparation method of a pitch-based universal-grade carbon fiber needled felt comprises the following steps:
1) preparation of the starting materials
The method for producing and preparing the pitch-based general-grade carbon fiber filament comprises the following steps:
firstly, heating the spun asphalt to 300 ℃, uniformly mixing under the action of an extruder, pressurizing to 1.5Mpa by a melt pump, and preparing asphalt protofilaments by a spinning die head;
secondly, the pitch protofilament is oxidized for 3 hours at the temperature of 150 ℃ by a pre-oxidation furnace to obtain pre-oxidized filaments;
③ sending the pre-oxidized fiber into a carbonization furnace, carbonizing at 900 deg.C for 3 hr in nitrogen atmosphere, and making into pitch-based universal carbon fiber precursor with carbon content not less than 93% and true density of 1.7-1.8g/cm3；
2) Opening in one step
Feeding the pitch-based general-grade carbon fiber filament prepared in the step 1) into an opener through a feeding roller, and preparing a 8 cm-long first-grade pitch-based general-grade carbon fiber short filament after the pitch-based general-grade carbon fiber filament is treated by a nail roller rotating at a high speed;
the rotating speed of the opener is 800 r/min, and the nails of the opener nail roller are tangent with the feeding material at an angle of 15-16 degrees; the length of the nails on the nail roller is 25mm, and the nail density of the nail roller is 0.2-0.3 per square centimeter;
3) secondary opening
Pumping the primary pitch-based general-grade carbon fiber short filaments prepared in the step 2) into a cotton box through a fan, and preparing secondary pitch-based general-grade carbon fiber short filaments with the length of 4cm through conveying a nail curtain and the action of front and rear nail rollers; opening parameters are the same as those of primary opening;
4) pre-needled felt preparation
Pumping the prepared second-stage asphalt-based general-grade carbon fiber short filament into a cotton dropping box through a fan, enabling the second-stage asphalt-based general-grade carbon fiber short filament to uniformly drop onto a cotton conveying curtain with the thickness of 6cm under the action of a polarizing plate and a star-horn discharging roller, enabling the second-stage asphalt-based general-grade carbon fiber short filament to enter a web forming box through the cotton conveying curtain, and enabling the asphalt-based general-grade carbon fiber short filament to uniformly drop onto the web forming box under the action of a high-speed nail roller and air flowOn the curtain, the laying gram weight is 500g/m2Entering a pre-needling machine through a net forming curtain to be needled into a pre-needled felt;
5) needling treatment
Conveying the pre-needled felt prepared in the step 4) to a needle machine again through a conveying and shaping mesh belt, carrying out needling treatment, sequentially carrying out forming treatment through a No. 2 needle machine and a No. 3 needle machine, and after the treatment is finished, carrying out edge cutting and shaping through a trimming machine, and then rolling and boxing.
Example 2
A preparation method of a pitch-based universal-grade carbon fiber needled felt comprises the following steps:
1) preparation of the starting materials
The method for producing and preparing the pitch-based general-grade carbon fiber filament comprises the following steps:
firstly, heating the spun asphalt to 280 ℃, uniformly mixing under the action of an extruder, pressurizing by a melt pump to 2.5Mpa, and preparing asphalt protofilaments through a spinning die head;
secondly, the pitch protofilament is oxidized for 2 hours at the temperature of 250 ℃ by a pre-oxidation furnace to obtain pre-oxidized filaments;
③ sending the pre-oxidized fiber into a carbonization furnace, carbonizing at 900 deg.C for 1.5h in nitrogen atmosphere, and making into pitch-based universal carbon fiber precursor with carbon content not less than 93% and true density of 2.0-2.1g/cm3；
2) Opening in one step
Feeding the pitch-based general-grade carbon fiber filament prepared in the step 1) into an opener through a feeding roller, and preparing a 10 cm-long first-grade pitch-based general-grade carbon fiber short filament after the pitch-based general-grade carbon fiber filament is treated by a nail roller rotating at a high speed;
the rotating speed of the opener is 750 revolutions per minute, and the nails of the opener nail roller are tangent with the feeding material at an angle of 16-20 degrees; the length of the nails on the nail roller is 28mm, and the nail density of the nail roller is 0.2-0.3 per square centimeter;
3) secondary opening
Pumping the primary pitch-based general-grade carbon fiber short filaments prepared in the step 2) into a cotton box through a fan, and preparing secondary pitch-based general-grade carbon fiber short filaments with the length of 4cm through conveying a nail curtain and the action of front and rear nail rollers; opening parameters are the same as those of primary opening;
4) pre-needled felt preparation
Pumping the prepared second-stage asphalt-based general-grade carbon fiber short filament into a cotton dropping box, uniformly dropping the second-stage asphalt-based general-grade carbon fiber short filament onto a cotton conveying curtain with the thickness of 7cm under the action of a polarizing plate and a star-horn discharging roller, feeding the second-stage asphalt-based general-grade carbon fiber short filament into a net forming box through the cotton conveying curtain, uniformly dropping the asphalt-based general-grade carbon fiber short filament onto the net forming curtain under the action of a high-speed nail roller and air flow, and laying the asphalt-based general-grade carbon fiber short filament with the grammage of 800g/m2Entering a pre-needling machine through a net forming curtain to be needled into a pre-needled felt;
5) needling treatment
Conveying the pre-needled felt prepared in the step 4) to a needle machine again through a conveying and shaping mesh belt, carrying out needling treatment, sequentially carrying out forming treatment through a No. 2 needle machine and a No. 3 needle machine, carrying out edge cutting and shaping through a trimming machine, and then rolling and boxing.
Example 3
A preparation method of a pitch-based universal-grade carbon fiber needled felt comprises the following steps:
1) preparation of the starting materials
The method for producing and preparing the pitch-based general-grade carbon fiber filament comprises the following steps:
firstly, heating the spun asphalt to 350 ℃, uniformly mixing under the action of an extruder, pressurizing to 1.0Mpa by a melt pump, and preparing asphalt protofilaments by a spinning die head;
secondly, the pitch protofilament is oxidized for 1.5 hours at the temperature of 450 ℃ by a pre-oxidation furnace to obtain pre-oxidized fiber;
③ sending the pre-oxidized fiber into a carbonization furnace, carbonizing at 1300 deg.C for 0.5 hr in nitrogen atmosphere, and making into pitch-based universal carbon fiber precursor with carbon content not less than 93% and true density of 1.4-1.5g/cm3；
2) Opening in one step
Feeding the pitch-based general-grade carbon fiber filament prepared in the step 1) into an opener through a feeding roller, and preparing a 12 cm-long first-grade pitch-based general-grade carbon fiber short filament after the pitch-based general-grade carbon fiber filament is treated by a nail roller rotating at a high speed;
the rotating speed of the opener is 700 revolutions per minute, and the nails of the opener nail roller are tangent with the feeding material at an angle of 15-25 degrees; the length of the nails on the nail roller is 30mm, and the nail density of the nail roller is 0.2-0.3 per square centimeter;
3) secondary opening
Pumping the primary pitch-based general-grade carbon fiber short filaments prepared in the step 2) into a cotton box through a fan, and preparing secondary pitch-based general-grade carbon fiber short filaments with the length of 5cm through conveying a nail curtain and the action of front and rear nail rollers; opening parameters are the same as those of primary opening;
4) pre-needled felt preparation
Pumping the prepared second-stage asphalt-based general-grade carbon fiber short filament into a cotton dropping box, uniformly dropping the second-stage asphalt-based general-grade carbon fiber short filament onto a cotton conveying curtain with the thickness of 8cm under the action of a polarizing plate and a star-horn discharging roller, feeding the second-stage asphalt-based general-grade carbon fiber short filament into a net forming box through the cotton conveying curtain, uniformly dropping the asphalt-based general-grade carbon fiber short filament onto the net forming curtain under the action of a high-speed nail roller and air flow, and paving the net forming box with the grammage of 1000g/m2Entering a pre-needling machine through a net forming curtain to be needled into a pre-needled felt;
5) needling treatment
Conveying the pre-needled felt prepared in the step 4) to a needle machine again through a conveying and shaping mesh belt, carrying out needling treatment, sequentially carrying out forming treatment through a No. 2 needle machine and a No. 3 needle machine, and after the treatment is finished, carrying out edge cutting and shaping through a trimming machine, and then rolling and boxing.
In the present application, the preparation of the pitch-based general-purpose carbon fiber filament refers to a method disclosed in an invention patent previously applied by the applicant, the application number is CN2012102345712, a method for preparing a spun pitch is not disclosed in the particular present application, and the present application is prepared according to the method for preparing the pitch with light components removed in the above prior application patent. The spun asphalt in the embodiment of the application is prepared by the following specific process method: circularly adding the medium-temperature pitch into a molecular distiller through a circulating pump, wherein the circulating rate is 520ml/min, the distillation is carried out under the conditions that the vacuum negative pressure is 0.05-0.07MPa, the distillation initial temperature is 155 ℃ and the distillation and condensation temperature difference is 55-58 ℃, the temperature is continuously increased in the distillation process, the temperature increasing rate is 3.5-4 ℃/min, when the distillation temperature is increased to 380 ℃, no obvious fraction is produced in the distiller, the distillation is stopped, and the low-QI coal pitch is obtained after residues are removed; under the conditions of 270 ℃ and 280 ℃, air is used as an oxidant to carry out oxidation treatment on the low-QI coal pitch, and the oxidation time is 8-9 h; and (3) carrying out thin-film distillation on the oxidized asphalt at the temperature of 335 ℃ and the vacuum negative pressure of 0.05-0.06MPa for 2-3h, and removing light components to obtain the spun asphalt.
The method for detecting the prepared asphalt-based universal carbon fiber filament comprises the following steps: detecting according to the method shown in GJB 1871-1994; the items tested included individual fiber tensile strength, tensile modulus, elongation at break, diameter measurements.
Example 1, example 2, and example 3 measured 10, 9, and 9 groups, respectively, and numbered 1 to 28 in this order, and the results are shown in table 1 below.
TABLE 1
Due to the adoption of the melt-blown method for production and preparation, the physical properties of part of the pitch-based general-grade carbon fiber filaments have large difference.
Comparative example 1
The same procedure as in example 2 was followed with only one opening.
A preparation method of a pitch-based universal-grade carbon fiber needled felt comprises the following steps:
1) preparation of the starting materials
The method for producing and preparing the pitch-based general-grade carbon fiber filament comprises the following steps:
1) heating the spun asphalt to 280 ℃, uniformly mixing under the action of an extruder, pressurizing by a melt pump to 2.5Mpa, and preparing asphalt protofilaments through a spinning die head;
2) carrying out oxidation treatment on the asphalt protofilament for 2 hours at the temperature of 250 ℃ by using a pre-oxidation furnace to obtain pre-oxidized filaments;
3) feeding the pre-oxidized fibers into a carbonization furnace, carbonizing at 900 ℃ for 1.5 hours in a nitrogen atmosphere, and preparing the pre-oxidized fibers into asphalt-based universal carbon fiber precursors; the carbon content of the produced asphalt-based universal carbon fiber precursor is more than or equal to 93 percent, and the true density is 2.0-2.1g/cm3；
2) Opening or shredding
Feeding the pitch-based general-grade carbon fiber filament prepared in the step 1) into an opener through a feeding roller, and preparing a 10 cm-long pitch-based general-grade carbon fiber short filament after the pitch-based general-grade carbon fiber filament is treated by a nail roller rotating at a high speed;
the rotating speed of the opener is 750 revolutions per minute, and the nails of the opener nail roller are tangent with the feeding material at an angle of 16-20 degrees; the length of the nails on the nail roller is 28mm, and the nail density of the nail roller is 0.2-0.3 per square centimeter;
3) pre-needled felt preparation
Pumping the prepared asphalt-based general-grade carbon fiber short filament into a cotton dropping box, uniformly dropping the second-grade asphalt-based general-grade carbon fiber short filament onto a cotton conveying curtain with the thickness of 7cm under the action of a polarizing plate and a star-horn discharging roller, then entering a net forming box through the cotton conveying curtain, uniformly dropping the asphalt-based general-grade carbon fiber short filament onto the net forming curtain under the action of a high-speed nail roller and air flow, and laying the asphalt-based general-grade carbon fiber short filament with the gram weight of 800g/m2Entering a pre-needling machine through a net forming curtain to be needled into a pre-needled felt;
4) needling treatment
Conveying the pre-needled felt prepared in the step 3) to a needle machine again through a conveying and shaping mesh belt, carrying out needling treatment, sequentially carrying out forming treatment through a No. 2 needle machine and a No. 3 needle machine, and after the treatment is finished, carrying out edge cutting and shaping through a trimming machine, and then rolling and boxing.
Comparative example 2
The rotating speed of the opener is 1000 r/min, and when the opening treatment is adopted for one time:
a preparation method of a pitch-based universal-grade carbon fiber needled felt comprises the following steps:
1) preparation of the starting materials
The method for producing and preparing the pitch-based general-grade carbon fiber filament comprises the following steps:
firstly, heating the spun asphalt to 280 ℃, uniformly mixing under the action of an extruder, pressurizing by a melt pump to 2.5Mpa, and preparing asphalt protofilaments through a spinning die head;
secondly, the pitch protofilament is oxidized for 2 hours at the temperature of 250 ℃ by a pre-oxidation furnace to obtain pre-oxidized filaments;
③ sending the pre-oxidized fiber into a carbonization furnace, carbonizing at 900 deg.C for 1.5h in nitrogen atmosphere, and making into pitch-based universal carbon fiber precursor with carbon content not less than 93% and true density of 2.0-2.1g/cm3；
2) Opening in one step
Feeding the pitch-based general-grade carbon fiber filament prepared in the step 1) into an opener through a feeding roller, and preparing a 10 cm-long first-grade pitch-based general-grade carbon fiber short filament after the pitch-based general-grade carbon fiber filament is treated by a nail roller rotating at a high speed;
the rotating speed of the opener is 1000 revolutions per minute, and the nails of the opener nail roller are tangent with the feeding material at an angle of 16-20 degrees; the length of the nails on the nail roller is 28mm, and the nail density of the nail roller is 0.2-0.3 per square centimeter;
3) pre-needled felt preparation
Pumping the prepared second-stage asphalt-based general-grade carbon fiber short filament into a cotton dropping box, uniformly dropping the second-stage asphalt-based general-grade carbon fiber short filament onto a cotton conveying curtain with the thickness of 7cm under the action of a polarizing plate and a star-horn discharging roller, feeding the second-stage asphalt-based general-grade carbon fiber short filament into a net forming box through the cotton conveying curtain, uniformly dropping the asphalt-based general-grade carbon fiber short filament onto the net forming curtain under the action of a high-speed nail roller and air flow, and paving the net forming box with the grammage of 1000g/m2Entering a pre-needling machine through a net forming curtain to be needled into a pre-needled felt;
4) needling treatment
Conveying the pre-needled felt prepared in the step 3) to a needle machine again through a conveying and shaping mesh belt, carrying out needling treatment, sequentially carrying out forming treatment through a No. 2 needle machine and a No. 3 needle machine, carrying out edge cutting and shaping through a trimming machine, and then rolling and boxing.
The pitch-based carbon fiber precursor is formed into short filaments of 3-5 cm in one-time opening, and the formed needled felt is cracked through the subsequent production in the same steps, so that the product quality is reduced, the heat conductivity is uneven, and the felt cannot be used by users.
The opener was rotated at 500 rpm and the rest of the procedure was the same as in example 2.
The rotating speed of the opener is 500 r/min, and under the condition that other parameters are not changed, the pitch-based carbon fiber protofilament cannot be chopped well, so that the formed super-filament is wound on the nail roller of the opener, and the production cannot be carried out.
Comparative example 3
The method is characterized by selecting commercially available polyacrylonitrile protofilaments for preparing the PAN-based graphite felt, wherein the polyacrylonitrile protofilaments selected in the method are purchased from Wuxi Weisheng New Material science and technology company Limited.
The preparation process of the PAN-based oxidized silk cured graphite felt comprises the following steps:
the method comprises the steps of preparing polyacrylonitrile protofilament, pre-oxidizing, felting, coating phenolic resin glue, multi-layer hot-pressing curing (4 cm thick), pre-carbonizing and graphitizing to finally obtain the PAN-based oxidized fiber cured graphite felt.
The preparation process of the PAN-based common cured graphite felt comprises the following steps:
the method comprises the steps of preparing polyacrylonitrile protofilament, felting, pre-oxidizing, coating phenolic resin glue, multi-layer hot-pressing curing (4 cm thick), pre-carbonizing and graphitizing to finally obtain the PAN-based common cured graphite felt.
The preparation process of the asphalt-based cured graphite felt comprises the following steps:
carbonized pitch-based needled felt carbon fiber precursor, needled felt, phenolic resin glue coating, multi-layer hot-pressing curing (4 cm thick), pre-carbonization and graphitization, and finally the pitch-based cured graphite felt is prepared.
The subsequent gluing, pre-carbonization and graphitization are carried out by the conventional technology disclosed in the prior art, and the gluing, pre-carbonization and graphitization processes of the PAN-based graphite felt in the embodiment and the comparative example are the same. When the same preparation steps are involved, the process parameters of the PAN-based graphite felt can be adaptively modified by referring to the parameters disclosed in the embodiments of the present application, that is, the asphalt-based graphite felt and the PAN-based graphite felt are prepared under the same or similar process parameter conditions and process steps.
The application further conducted thermal insulation tests on the performance of graphite felt produced using needle punched felt as described in examples 1-3, comparative example 1, and comparative example 3.
1 part of each of the samples of examples 1-3, comparative example 1 and comparative example 3 is taken, the samples are processed into graphite felts with the same specification according to the requirements, and the graphite felts are subjected to high-temperature treatment at the temperature of over 1800 ℃ and have the performance compared with polyacrylonitrile carbon fiber needled felts.
TABLE 2
The foregoing is illustrative of the preferred embodiments of this invention, and it is to be understood that the invention is not limited to the precise form disclosed herein and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the concept as disclosed herein, either as described above or as apparent to those skilled in the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The preparation method of the asphalt-based general-grade carbon fiber needled felt is characterized by comprising the following steps of:
1) preparation of the starting materials
Preparing asphalt-based general-grade carbon fiber filaments for later use;
2) opening in one step
Feeding the pitch-based general-grade carbon fiber filament prepared in the step 1) into an opener through a feeding roller to prepare a first-grade pitch-based general-grade carbon fiber short filament;
3) secondary opening
Conveying the primary pitch-based universal carbon fiber short filaments prepared in the step 2) into a cotton box by wind, and preparing secondary pitch-based universal carbon fiber short filaments under the action of a conveying nail curtain;
4) pre-needled felt preparation
Conveying the second-stage pitch-based general-grade carbon fiber short filaments prepared in the step 3) into a cotton dropping box, uniformly paving the second-stage pitch-based general-grade carbon fiber short filaments on a cotton conveying curtain, then placing the cotton conveying curtain on a net forming box, uniformly paving the cotton conveying curtain on a net forming curtain, and preparing a pre-punched felt under the action of a pre-punching machine;
5) needling treatment
And (3) carrying out multistage needling treatment on the pre-punched felt prepared in the step (4), and then carrying out edge cutting and rolling.
2. The method for preparing the pitch-based general-purpose carbon fiber needled felt according to claim 1, characterized in that: 1) in the preparation of raw materials, the method for preparing the pitch-based universal-grade carbon fiber filament comprises the following steps:
firstly, heating the spun asphalt to the temperature of 280 ℃ and 350 ℃, pressurizing to 1-2.5Mpa by a melt pump, and preparing asphalt protofilaments by a spinning die head;
secondly, the pitch protofilament is oxidized in a pre-oxidation furnace at the temperature of 150 ℃ and 450 ℃ to obtain pre-oxidized fiber;
thirdly, the pre-oxidized fiber is sent into a carbonization furnace, and the pre-oxidized fiber is prepared into the pitch-based universal carbon fiber precursor at the temperature of over 900 ℃ in the nitrogen atmosphere.
3. The method for preparing the pitch-based general-purpose carbon fiber needled felt according to claim 2, characterized in that: the diameter of the pitch-based universal carbon fiber precursor is 5-15 mu m, the carbon content is more than or equal to 93 percent, and the density is 1.4-2.3g/cm3。
4. The method for preparing the pitch-based general-purpose carbon fiber needled felt according to claim 1, characterized in that: 2) in the primary opening, the length of the primary asphalt base general-grade carbon fiber short filament is 8-12 cm.
5. The method for preparing the pitch-based general-purpose carbon fiber needled felt according to claim 1, characterized in that: 3) in the secondary opening, the length of the second-level asphalt-based general-level carbon fiber short filament is 4-5 cm.
6. The method for preparing the pitch-based general-purpose carbon fiber needled felt according to claim 1, characterized in that: the rotating speed of the opener is 700-800 rpm, and the nails of the nail roller of the opener are tangent to the feeding material at an angle of 15-25 ℃; the length of the nails on the nail roller is more than or equal to 25mm, and the nail density of the nail roller is 0.2-0.3 per square centimeter.
7. The method for preparing the pitch-based general-purpose carbon fiber needled felt according to claim 1, characterized in that: 4) in the preparation of the pre-punched felt, the pre-punched felt is uniformly paved on a cotton conveying curtain with the thickness of 6-8 cm; the laying gram weight is 500-1000g/m2。
8. The utility model provides a general grade carbon fiber needled felt of pitch base which characterized in that: the asphalt-based general-grade carbon fiber needled felt is prepared by the preparation method of the asphalt-based general-grade carbon fiber needled felt according to any one of claims 1 to 7.
9. Use of a pitch-based universal grade carbon fiber needled felt according to claim 8, wherein: used as a heat preservation article in the process of producing and preparing crystal silicon products.
10. Use of a pitch-based universal grade carbon fiber needled felt according to claim 9, characterized in that: the crystalline silicon product comprises photovoltaic crystalline silicon and semiconductor chip crystalline silicon.
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| CN114232215A (en) * | 2021-12-20 | 2022-03-25 | 西安工程大学 | Preparation method and application of asphalt-based carbon nanofiber multistage non-woven fabric with three-dimensional cavity structure |
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