CN113293640B - Para-aramid nanofiber and high-performance carbon fiber composite paper and preparation method thereof - Google Patents
Para-aramid nanofiber and high-performance carbon fiber composite paper and preparation method thereof Download PDFInfo
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- CN113293640B CN113293640B CN202110717099.7A CN202110717099A CN113293640B CN 113293640 B CN113293640 B CN 113293640B CN 202110717099 A CN202110717099 A CN 202110717099A CN 113293640 B CN113293640 B CN 113293640B
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP 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
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/36—Inorganic fibres or flakes
- D21H13/46—Non-siliceous fibres, e.g. from metal oxides
- D21H13/50—Carbon fibres
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP 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
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/54—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen
- D21H17/55—Polyamides; Polyaminoamides; Polyester-amides
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP 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
- D21H21/00—Non-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
- D21H21/06—Paper forming aids
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP 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
- D21H21/00—Non-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
- D21H21/06—Paper forming aids
- D21H21/08—Dispersing agents for fibres
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP 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
- D21H23/00—Processes or apparatus for adding material to the pulp or to the paper
- D21H23/02—Processes or apparatus for adding material to the pulp or to the paper characterised by the manner in which substances are added
- D21H23/22—Addition to the formed paper
- D21H23/50—Spraying or projecting
Abstract
The invention belongs to the field of papermaking technology and materials, and particularly relates to para-aramid nanofiber and high-performance carbon fiber composite paper and a preparation method thereof. The method has the advantages that the characteristics of large specific surface area of para-aramid nanofibers, easy dispersion in aqueous solution and the like are utilized, the traditional slurry wet strength agent and adhesive can be replaced, the fully and uniformly mixed with high-performance carbon fiber solution is realized, wet paper sheets of para-aramid fibers and carbon fibers are prepared through wet paper making, then para-aramid nanofiber dispersion liquid is sprayed and sized on the surfaces of the wet paper sheets of the aramid fibers, then composite drying and forming are carried out, and the sprayed and compounded paper sheets can remarkably improve the uniformity and mechanical strength of composite paper, improve the production efficiency of composite paper base materials and the like, and can fully realize the compounding of the carbon fibers and the aramid fibers. The composite material prepared by the method has good heat resistance, chemical stability and excellent heat conduction and electric conduction performance.
Description
Technical Field
The invention belongs to the technical field of papermaking, and particularly relates to para-aramid nanofiber and high-performance carbon fiber composite paper and a preparation method thereof.
Background
In recent years, research and application of high-performance materials are rapidly developed, and aramid fiber is also increasingly receiving attention as a novel synthetic fiber material with high strength, high modulus and high temperature resistance. The aramid paper prepared from the aramid fibers through the papermaking process has excellent dielectric property, mechanical property, high temperature resistance, chemical corrosion resistance and flexible designability. The carbon fiber has the advantages of light weight, high specific strength, high temperature resistance, corrosion resistance and the like, and has great development potential in the development of high-speed trains. Both fibers are widely applied to the fields of aerospace, rail transit and the like, are key materials for realizing light weight and high speed, and are increasingly widely applied to the field of high-performance composite materials. The upgrade of the rapid prototyping technology for preparing the high-performance paper-based composite material by combining the aramid fiber and the carbon fiber needs to be further improved.
The composite material of the high-performance fiber paper-based material has overall performance superior to that of a single fiber material, and the advantages of different fiber materials can be fully exerted. The aramid fiber is a high-performance fiber material with high strength, high modulus, light weight, folding resistance, high temperature resistance, flame retardance and corrosion resistance, but has the characteristics of difficult heat conduction, easy flocculation, difficult dispersion and the like; the carbon fiber has the advantages of high strength, high modulus, corrosion resistance, good heat stability, low elongation at break, poor binding force between fibers during compounding, easy brittle failure and the like.
The para-aramid nanofiber has large specific surface area, is uniformly dispersed in the water phase and does not self-polymerize. The method has the characteristics of easy molding, good wet processing performance and excellent composite reinforcing effect when preparing the aramid paper, and avoids the problems of stiff pulp fiber form, loose paper bonding, poor performance and the like in the conventional aramid paper making process, thereby being better suitable for preparing the composite paper.
The strength of the carbon fiber composite material mainly depends on the binding force between the carbon fiber and the composite material, the specific surface area of the para-aramid nanofiber is large, the dispersing agent and the binder can be used in the slurry, the binding force between the fibers of the composite material can be effectively improved, the internal binding void ratio of the composite material is reduced, and the binding compactness is improved, so that the overall performance of the composite material is improved.
The preparation method of the para-aramid nanofiber and high-performance carbon fiber composite material paper is characterized in that chopped fibers of carbon fibers are used as a reinforcement, and the para-aramid nanofiber is used as a matrix, so that the composite material is prepared through a modern papermaking wet papermaking and hot-press molding process, overcomes the defects of untight combination, easiness in layering and the like caused by bonding of aramid paper and carbon fiber paper, is a high-performance composite material with excellent high strength, high modulus, light weight, high temperature resistance, flame retardance and corrosion resistance, can be widely applied to high-tech fields such as aerospace, rail transit, electronic and electric, national defense and military industry and the like as a structural material and an electronic material, and has a broad market prospect.
Disclosure of Invention
The invention provides para-aramid nanofiber and high-performance carbon fiber composite paper and a preparation method thereof. According to the invention, the characteristics of large specific surface area of para-aramid nanofiber, easy dispersion in aqueous solution and the like are utilized, the traditional slurry wet strength agent and adhesive can be replaced, the fully and uniform mixing with high-performance carbon fiber solution is realized, wet paper sheets of para-aramid fiber and carbon fiber are prepared through wet papermaking, then the para-aramid nanofiber dispersion liquid is subjected to spraying sizing treatment on the surface of the wet paper sheets, and then composite drying forming is carried out, so that the sprayed and compounded paper sheets can remarkably improve the uniformity and mechanical strength of composite paper, the production efficiency of composite paper-based materials and the like, and the compounding of carbon fiber and aramid fiber can be fully realized. The composite material prepared by the method has good heat resistance, chemical stability and excellent heat conduction and electric conduction performance.
The technical scheme adopted by the invention is as follows:
a para-aramid nanofiber and high-performance carbon fiber composite paper and a preparation method thereof are provided, wherein the raw material components comprise high-performance carbon fibers and para-aramid nanofibers.
The preparation method comprises the following steps:
1) And (3) preparing a component A: dispersing carbon fibers in deionized water through a high-frequency carding device, wherein the mass dispersion concentration of the carbon fibers is 0.001% -0.1%, and adding a dispersing agent and a surfactant, so that the carbon fibers are required to be fully and uniformly dispersed;
2) And (3) preparing a component B: dispersing para-aramid nanofibers into dispersion liquid by deionized water, and adjusting the mass dispersion concentration to be 0.05-0.5%, wherein the mass dispersion concentration is required to be fully and uniformly dispersed;
3) Mixing the component A and 70-95% of the component B according to the proportion, placing the mixture into a pulp mixing kettle for pulp mixing, adjusting the pulp concentration to be 0.005-0.2% by adding deionized water, and making the prepared pulp into a paper-based wet paper sheet;
4) When the composite slurry is formed in a suction filtration mode at the net part, the residual component B is subjected to single-sided uniform spraying on the upper surface of the composite paper base material in a compression spraying mode, and a layer of compact uniform para-aramid nanofiber film is formed on the upper surface of the composite paper. By the method, the problem of uneven distribution of the upper layer and the lower layer of the component B during suction filtration can be solved, and meanwhile, the uniformity of the surface layer can be ensured.
5) And squeezing, drying and hot-pressing the wet paper sheet to obtain the composite paper-based material.
Before the component A in the step 1) is prepared, the following steps are carried out: carrying out surface treatment on the slurry carbon fiber: carrying out high-temperature etching treatment on the carbon fiber in a muffle furnace at a high temperature of 350-450 ℃, and preferably 400 ℃; the treatment time is 0.5 to 2 hours, preferably 1 hour; during operation, attention is paid to temperature control, and when the temperature is too high, the strength of the carbon fiber is reduced, and when the temperature is too low, the treatment effect is not obvious. The treated carbon fiber can remove the auxiliary agent on the surface of the carbon fiber, increase the surface area of the carbon fiber, improve the dispersibility of the carbon fiber in water, provide more connecting points for the lap joint between the carbon fiber and the aramid fiber, and avoid the influence of other components caused by solvent treatment.
Adding a dispersing agent and a surfactant when the component A in the step 1) is subjected to high-frequency fluffing, wherein the dosage of the dispersing agent is 0.5-10% of the mass of the carbon fiber, and preferably 3-8%; the dosage of the surfactant is 1-10% of the mass of the carbon fiber, preferably 5-6%; the fluffer frequency is 5000-20000 r/min, preferably 10000-15000 r/min; the fluffing time is preferably 3-5 min. In the operation, the stability of the dispersion system is properly improved through the addition of the auxiliary agent, so that different fibers can be uniformly dispersed, and the net part forming is facilitated. Preferably, the dispersing agent consists of polyethylene oxide (PEO) and Polyacrylamide (PAM) with a mass ratio of 3:1.
Preferably, the dispersion concentration of the carbon fiber in the step 1) is 0.01-0.08%;
preferably, the dispersion concentration of the para-aramid nanofibers in the step 2) is 0.1% -0.3%.
In the invention, the component A accounts for 0.5 to 30 percent of the absolute dry weight percentage of the fiber, and the component B accounts for the balance; preferably 10% -20% of component A and the balance of component B.
In the step 3), the amount of the component B is 70-95% of the mass of the whole component B, preferably 80-90% based on the absolute dry weight of the fiber. The remaining component B is used for spraying in the step 4), the spraying amount is strictly controlled during operation, and too small can cause discontinuous film formation and too high, so that the component B and the underlying substrate are delaminated during subsequent hot pressing.
Preferably, the mesh number of the papermaking filter screen in the step 4) is 100-300 meshes.
Preferably, the vacuum degree in the vacuum suction dehydration process in the step 5) is kept between 0.015 and 0.05MPa, and the dryness after the vacuum suction dehydration is controlled between 6 and 15 percent.
Step 5) squeezing under the pressure of 2-5 MPa; drying at 130-160 deg.c for 3-10 min, high temperature polishing, hot pressing in hot press at 5-15 MPa and 100-300 deg.c for 1 times. The hot pressing temperature is preferably 200 to 300 ℃.
Preferably, the diameter of the component B fiber is 10-200 nm.
Preferably, the length of the component A fiber is 5-12 mm, and the diameter is 5-8 mu m.
The beneficial effects of the invention are as follows:
the invention utilizes high temperature to treat the carbon fiber, can eliminate the carbon fiber surface oiling agent, can generate deeper nicks on the surface of the carbon fiber, and can increase the surface area of the fiber. Although carbon fiber is connected by nonpolar covalent bond, the carbon fiber has few surface active groups, is not easy to be wetted by water, improves the number of the surface active groups of the fiber by etching, increases the combination opportunity of the carbon fiber, a dispersing agent and a surfactant, and is favorable for dispersing in medium water.
The para-aramid nanofiber not only has the excellent performances of high strength, high modulus, light weight, folding resistance, high temperature resistance, flame retardance and corrosion resistance of the para-aramid fiber, but also has the advantages of uniform dispersion in water, large specific surface area, no self-aggregation and the like, and has the characteristics of easy molding, good wet processing performance and excellent composite reinforcing effect when being used for preparing aramid paper.
More importantly, para-aramid nanofibers are added into the composite paper in two steps, and most of para-aramid nanofibers are directly added into the paper as slurry components, so that the combination property with carbon fibers is improved, the support and connection in the paper are enhanced, and the paper forming property is enhanced on the basis; and then, spraying and reinforcing treatment is carried out on the paper sheet by utilizing a small part of para-aramid nanofiber dispersion liquid, and the para-aramid nanofiber dispersion liquid is compounded on the wet paper sheet by a net part in a spraying manner, so that the characteristics of large specific surface area, good compatibility and excellent filling effect of the nanofibers can be brought into play, gaps of the paper sheet are filled, acting force among the fibers is enhanced, and the overall performance of the composite paper can be improved. The technology can improve the production efficiency and effectively ensure the overall performance of the aramid paper under the condition of ensuring the density and the uniformity of the finished paper.
In conclusion, the invention adopts the new technology and the new method to develop and produce the high-performance composite paper, has strong innovation and wide application prospect, and has great practical significance for promoting the development of the high-technology industry, promoting the upgrading and updating of the traditional industry, promoting the grade of products such as high-strength special paper and the like and promoting the development of related industries.
Detailed Description
The above-described aspects of the present invention will be described in further detail by way of the following embodiments, but it should not be construed that the scope of the above-described subject matter of the present invention is limited to the following examples. All techniques implemented based on the above description of the invention are within the scope of the invention. The following examples were carried out using conventional techniques, except as specifically described.
The detection criteria adopted for the embodiment of the invention are as follows:
the quantitative use of the paper sample is GB T451.2-2002 'quantitative determination of paper and paper board';
the thickness of the paper sample adopts GB T451.3-2002 'determination of the thickness of paper and paper board';
the tensile strength and the elongation of the paper sample adopt GBT 12914-2008 'determination of tensile strength of paper and paper board';
the tearing strength of the paper sample is measured by GB/T455-2002;
the air permeability of the paper sample adopts GBT 458-2008 'determination of air permeability of paper and paper board';
the component A adopted in the following embodiment of the invention is market purchased fiber aramid carbon fiber, the preparation of the component B para-aramid nanofiber adopts the prior art, and particularly can adopt the patent technology of patent 'preparation method of para-aramid nanofiber' (application number 2015106244606).
The dispersants used in the examples below were each composed of polyethylene oxide (PEO) and Polyacrylamide (PAM) in a mass ratio of 3:1.
The adopted surfactants are sodium dodecyl benzene sulfonate.
Example 1
The para-aramid nanofiber and high-performance carbon fiber composite paper comprises the following raw material components of a component A and a component B, wherein the mass ratio of the component A to the component B is 30 according to the absolute dry weight of the fiber: 70.
(1) Surface treatment of carbon fiber (length 6 mm): carrying out high-temperature etching treatment on the carbon fiber in a muffle furnace at a high temperature of 400 ℃ for 1 hour, and cooling the carbon fiber for later use;
(2) And (3) preparing a component A: dispersing carbon fibers in deionized water through a high-frequency carding device, and adjusting the concentration to 0.1% in a dispersing way; wherein the dosage of the dispersing agent is 1% of the mass of the carbon fiber, and the dosage of the surfactant is 9% of the mass of the carbon fiber; fluffer frequency 8000r/min; the fluffing time is 5min;
(3) Component B (average diameter 10-200 nm) is prepared: dispersing the component B into a dispersion liquid by deionized water, wherein the dispersion concentration is 0.05%;
(4) Mixing the component A and 80% of the component B according to the proportion, placing the mixture into a pulp mixing kettle for pulp mixing, adjusting the pulp concentration to be 0.007%, and making the prepared pulp into aramid wet paper;
(5) And (3) uniformly spraying the residual component B on the upper surface of the composite aramid paper-based material in a single-sided manner by a compression spraying manner, and then carrying out vacuum suction dehydration on the bottom surface to form the composite wet paper sheet. Basis weight of paper 38g/m 2 The mesh number of the papermaking filter screen is 150 meshes.
(6) The wet paper sheet is vacuumized to remove water through the lower layer, the vacuum degree is 0.015Mpa-0.03Mpa, and the dryness is maintained to be more than 13%. The composite paper sheet is separated from the forming wire by vacuum suction and transferred to a press section for press dewatering. The water content of the wet paper sheet is removed by adopting a double-roller double-blanket three-way press, and the press pressure is 2.5 MPa, 3.5 MPa and 4.5MPa in sequence.
(7) And drying the pressed paper sheet by adopting an electric heating roller at the temperature of 140 ℃ for 7min to obtain a dried aramid paper finished product.
(8) And (3) carrying out high-temperature calendaring treatment on the paper sample prepared in the step (7), carrying out hot pressing on the paper sample on a hot press, controlling the pressure at 15MPa, controlling the hot pressing temperature at 200 ℃ and carrying out hot pressing for 1 time to obtain the composite reinforced aramid paper.
(9) Through test, the thickness of the para-aramid nanofiber and high-performance carbon fiber composite material paper is 0.05mm, and the ration is 38.5g/m 2 The average tensile strength was 2.3kN/m, the tearing strength was 1360mN, and the air permeability was 0.06 μm/Pa.S.
Example 2
The para-aramid nanofiber and high-performance carbon fiber composite paper comprises the following raw material components of a component A and a component B, wherein the mass ratio of the component A to the component B is 25 according to the absolute dry weight of the fiber: 75.
(1) Surface treatment of carbon fiber (length 7 mm): the treatment is carried out at a high temperature of 450 ℃ for 0.5 hour, and the treatment is cooled for standby.
(2) And (3) preparing a component A: dispersing carbon fiber in deionized water by a high-frequency carding machine, and adjusting the concentration to 0.01%. Wherein the dosage of the dispersing agent is 3% of the mass of the carbon fiber, and the dosage of the surfactant is 6% of the mass of the carbon fiber; the fluffer frequency is 10000r/min; the fluffing time is 5min;
(3) Component B (average diameter 10-200 nm) is prepared: component B was dispersed in deionized water to a dispersion concentration of 0.1%.
(4) Mixing the component A and 85% of the component B (85% of the total amount of the component) according to the proportion, placing the mixture into a pulp mixing kettle for pulp mixing, adjusting the pulp concentration to 0.025%, and making the prepared pulp into aramid wet paper.
(5) And (3) uniformly spraying the residual component B on the upper surface of the composite aramid paper-based material in a single-sided manner by a compression spraying manner, and then carrying out vacuum suction dehydration on the bottom surface to form the composite wet paper sheet. Basis weight of paper 40g/m 2 The mesh number of the papermaking filter screen is 150 meshes.
(6) The wet paper sheet is vacuumized to remove water through the lower layer, the vacuum degree is 0.02Mpa-0.04Mpa, and the dryness is maintained to be more than 11%. The composite paper sheet is separated from the forming wire by vacuum suction and transferred to a press section for press dewatering. The water content of the wet paper sheet is removed by adopting a double-roller double-blanket three-way press, and the press pressure is 2.5 MPa, 3.0 MPa and 4.0MPa in sequence.
(7) And drying the pressed paper sheet by adopting an electric heating roller at the temperature of 150 ℃ for 5min to obtain a dried aramid paper finished product.
(8) And (3) carrying out high-temperature calendaring treatment on the paper sample prepared in the step (7), carrying out hot pressing on the paper sample on a hot press, controlling the pressure at 9MPa, and carrying out hot pressing for 1 time at the hot pressing temperature of 250 ℃ to obtain the composite reinforced aramid paper.
(9) Through test, the thickness of the paper of the para-aramid nanofiber and high-performance carbon fiber composite material is 0.056mm, and the ration is 40.5g/m 2 The average tensile strength was 2.5kN/m, the tearability was 1637mN, and the air permeability was 0.05. Mu.m/Pa.S.
Example 3
The para-aramid nanofiber and high-performance carbon fiber composite paper comprises the following raw material components of a component A and a component B, wherein the mass ratio of the component A to the component B is 20 according to the absolute dry weight of the fiber: 80.
(1) Surface treatment of carbon fiber (length 8 mm): treating at 420 ℃ for 0.8 hour, and cooling for later use;
(2) And (3) preparing a component A: dispersing carbon fibers in deionized water through a high-frequency carding machine, and adjusting the concentration to 0.05%; wherein the dosage of the dispersing agent is 6% of the mass of the carbon fiber, and the dosage of the surfactant is 5% of the mass of the carbon fiber; the fluffer frequency is 15000r/min; the fluffing time is 4min;
(3) Component B (average diameter 10-200 nm) is prepared: dispersing the component B into a dispersion liquid by deionized water, wherein the dispersion concentration is 0.2%;
(4) Mixing the component A and the component B (87% of the total amount of the component) according to the proportion, placing the mixture into a pulp mixing kettle for pulp mixing, adjusting the pulp concentration to 0.1%, and making the prepared pulp into aramid wet paper;
(5) And (3) uniformly spraying the residual component B on the upper surface of the composite aramid paper-based material in a single-sided manner by a compression spraying manner, and then carrying out vacuum suction dehydration on the bottom surface to form the composite wet paper sheet. Basis weight of paper 41g/m 2 The mesh number of the papermaking filter screen is 200 meshes.
(6) The wet paper sheet is vacuumized to remove water through the lower layer, the vacuum degree is 0.03Mpa-0.05Mpa, and the dryness is maintained to be more than 8%. The composite paper sheet is separated from the forming wire by vacuum suction and transferred to a press section for press dewatering. The water content of the wet paper sheet is removed by adopting double-roller double-blanket three-way pressing, and the pressing pressure is sequentially 2.0 MPa, 3.0 MPa and 4.0MPa.
(7) And drying the pressed paper sheet by adopting an electric heating roller at 160 ℃ for 4min to obtain a dried aramid paper finished product.
(8) And (3) carrying out high-temperature calendaring treatment on the paper sample prepared in the step (7), carrying out hot pressing on the paper sample on a hot press, controlling the pressure at 12MPa, controlling the hot pressing temperature at 220 ℃ and carrying out hot pressing for 1 time to obtain the composite reinforced aramid paper.
(9) Through test, the thickness of the paper of the para-aramid nanofiber and high-performance carbon fiber composite material is 0.055mm, and the ration is 40.8g/m 2 The average tensile strength was 3.1kN/m, the tearing strength was 1587mN, and the air permeability was 0.03. Mu.m/Pa.S.
Example 4
The para-aramid nanofiber and high-performance carbon fiber composite paper comprises the following raw material components of a component A and a component B, wherein the mass ratio of the component A to the component B is 10 according to the absolute dry weight of the fiber: 90.
(1) Surface treatment of carbon fiber (length 10 mm): treating at a high temperature of 350 ℃ for 2 hours, and cooling for later use after the treatment is completed;
(2) And (3) preparing a component A: dispersing carbon fibers in deionized water through a high-frequency carding machine, and adjusting the concentration to 0.003%; wherein the dosage of the dispersing agent is 9% of the mass of the carbon fiber, and the dosage of the surfactant is 2% of the mass of the carbon fiber; the fluffer frequency is 20000r/min; the fluffing time is 3min;
(3) Component B (average diameter 10-200 nm) is prepared: dispersing the component B into a dispersion liquid by deionized water, wherein the dispersion concentration is 0.3%;
(4) Mixing the component A and 90% of the component B (90% of the total amount of the component) according to the proportion, placing the mixture into a pulp mixing kettle for pulp mixing, adjusting the pulp concentration to 0.2%, and making the prepared pulp into aramid wet paper;
(5) And (3) uniformly spraying the residual component B on the upper surface of the composite aramid paper-based material in a single-sided manner by a compression spraying manner, and then carrying out vacuum suction dehydration on the bottom surface to form the composite wet paper sheet. Basis weight of sheets 42g/m 2 The mesh number of the papermaking filter screen is 300 meshes.
(6) The wet paper sheet is vacuumized to remove water through the lower layer, the vacuum degree is 0.035Mpa-0.05Mpa, and the dryness is maintained to be more than 6%. The composite paper sheet is separated from the forming wire by vacuum suction and transferred to a press section for press dewatering. The water content of the wet paper sheet is removed by adopting double-roller double-blanket three-way pressing, and the pressing pressure is sequentially 2.5 MPa, 3.5 MPa and 5.0MPa.
(7) And drying the pressed paper sheet by adopting an electric heating roller at 130 ℃ for 10min to obtain a dried aramid paper finished product.
(8) And (3) carrying out high-temperature calendaring treatment on the paper sample prepared in the step (7), carrying out hot pressing on the paper sample on a hot press, controlling the pressure at 5MPa, controlling the hot pressing temperature at 300 ℃ and carrying out hot pressing for 1 time to obtain the composite reinforced aramid paper.
(9) Through test, the thickness of the para-aramid nanofiber and high-performance carbon fiber composite material paper is 0.06mm, and the ration is 42.8g/m 2 The average tensile strength was 3.5kN/m, the tearing strength was 1537mN, and the air permeability was 0.02 μm/Pa.S.
The present invention is not limited to the above embodiments, and any other modifications, adaptations, simplifications, combinations, and alternatives without departing from the spirit and principles of the invention are within the scope of the patent.
Claims (7)
1. The para-aramid nanofiber and high-performance carbon fiber composite paper is characterized by comprising the following raw material components of high-performance carbon fibers and para-aramid nanofibers, wherein the preparation method comprises the following steps:
1) And (3) preparing a component A: dispersing carbon fibers in deionized water, wherein the mass dispersion concentration of the carbon fibers is 0.001% -0.1%;
2) And (3) preparing a component B: dispersing para-aramid nanofibers into dispersion liquid by deionized water, and adjusting the mass dispersion concentration to 0.05% -0.5%;
3) Mixing the component A and 70-95% of the component B, placing the mixture into a pulp mixing kettle for pulp mixing, adjusting the pulp concentration to 0.005-0.2% by adding deionized water, and making the prepared pulp into a paper-based material wet paper sheet;
4) When the composite slurry is formed in a suction filtration mode at a net part, the residual component B is subjected to single-sided uniform spraying on the upper surface of a composite paper base material in a compression spraying mode, and then is subjected to vacuum suction dehydration through a bottom surface to form a composite wet paper sheet, and a layer of compact uniform para-aramid nanofiber film is formed on the upper surface of the composite paper;
5) Squeezing, drying and hot-pressing the wet paper sheet to obtain a composite paper-based material;
the component A accounts for 0.5 to 30 percent of the absolute dry weight percentage of the fiber, and the component B accounts for the balance;
the diameter of the component B fiber is 10-200 nm; the length of the component A fiber is 5-12 mm, and the diameter is 5-8 mu m;
before the component A in the step 1) is prepared, the following steps are carried out: surface treatment is carried out on the carbon fiber: carrying out high-temperature etching treatment on the carbon fiber in a muffle furnace at a high temperature of 350-450 ℃ for 0.5-2 hours;
adding a dispersing agent and a surfactant when the component A in the step 1) is dispersed, wherein the dosage of the dispersing agent is 0.5-10% of the mass of the carbon fiber; the dosage of the surfactant is 1-10% of the mass of the carbon fiber; the dispersing agent consists of polyethylene oxide (PEO) and Polyacrylamide (PAM), and the mass ratio of the dispersing agent to the polyacrylamide is 3:1;
in the step 3), the dosage of the component B is 70-95% of the mass of the whole component B according to the absolute dry weight of the fiber.
2. The para-aramid nanofiber and high-performance carbon fiber composite paper according to claim 1, wherein the component A is 10% -20% and the component B is the rest according to the absolute dry weight percentage of fibers.
3. The para-aramid nanofiber and high-performance carbon fiber composite paper according to claim 1, wherein when the component A in the step 1) is dispersed, the frequency of the high-frequency fluffer is 5000-20000 r/min; the fluffing time is 3-5 min.
4. The para-aramid nanofiber and high-performance carbon fiber composite paper according to claim 1, wherein the dispersion concentration of the carbon fibers in the step 1) is 0.01% -0.08%; the dispersion concentration of the para-aramid nanofibers in the step 2) is 0.1% -0.3%.
5. The para-aramid nanofiber and high-performance carbon fiber composite paper according to claim 1, wherein the vacuum degree in the vacuum suction dehydration process in the step 4) is kept between 0.015 and 0.05MPa, and the dryness after the vacuum suction dehydration is controlled between 6% and 15%.
6. The para-aramid nanofiber and high-performance carbon fiber composite paper according to claim 1, wherein the step 5) is pressed under a pressure of 2-5 MPa; drying at 130-160 deg.c for 3-10 min, high temperature polishing, hot pressing in hot press at 5-15 MPa and 100-300 deg.c for 1 times.
7. The para-aramid nanofiber and high-performance carbon fiber composite paper according to claim 1, wherein the mesh number of the papermaking filter screen in the step 3) is 100-300 meshes.
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