CN114836900B - Superfine viscose-based carbon fiber heat insulation hard felt and preparation method thereof - Google Patents
Superfine viscose-based carbon fiber heat insulation hard felt and preparation method thereof Download PDFInfo
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- 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
- D04H1/425—Cellulose series
- D04H1/4258—Regenerated cellulose series
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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
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
- D04H1/43838—Ultrafine fibres, e.g. microfibres
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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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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
- D06C7/04—Carbonising or oxidising
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/34—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxygen, ozone or ozonides
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
- D06M11/64—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/80—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides
- D06M11/82—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides with boron oxides; with boric, meta- or perboric acids or their salts, e.g. with borax
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/402—Amides imides, sulfamic acids
- D06M13/432—Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
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Abstract
The invention belongs to the technical field of heat insulation materials, and provides an ultrafine viscose-based carbon fiber heat insulation hard felt and a preparation method thereof, wherein the preparation method comprises the following steps: performing needling treatment on the superfine viscose fibers to obtain superfine viscose-based fiber mats; sequentially centrifuging and drying the superfine viscose-based fiber felt after being immersed in a catalyst system, and pre-oxidizing the dried product to obtain a pre-oxidized superfine viscose-based fiber felt; and (3) immersing the pre-oxidized superfine viscose-based fiber felt in a phenolic resin solution, curing, and carbonizing a cured product to obtain the superfine viscose-based carbon fiber heat-insulating hard felt. The superfine viscose-based carbon fiber heat insulation hard felt effectively improves the heat insulation performance of the carbon felt, prolongs the service life, and improves the mechanical property of the carbon felt after phenolic resin impregnation treatment. The thermal conductivity of the superfine viscose carbon fiber hard felt is 0.03-0.18W/m.k, and the tensile strength is 800-1050 MPa.
Description
Technical Field
The invention relates to the technical field of heat insulation materials, in particular to an ultrafine viscose-based carbon fiber heat insulation hard felt and a preparation method thereof.
Background
The temperature in the high temperature vacuum furnace is generally above 1350 ℃, for example, the solar silicon crystal needs to be grown at 1500 ℃ or above, and many high temperature crystal treatments are also above 1500 ℃. Conventional insulation cannot withstand such high temperatures, and therefore a suitable insulation needs to be found. The carbon felt has the characteristics of high temperature resistance, low heat capacity, energy conservation, durability, no pollution and the like, is particularly suitable for being used as a high-temperature heat insulation material because of the high-temperature resistance and the thermal field heat insulation requirement of high-temperature crystal growth, and can be widely applied to high-temperature heat insulation environments such as a solar polycrystalline silicon furnace, a monocrystalline silicon furnace, a semiconductor furnace, a sapphire furnace, a wire drawing furnace, a high-end metallurgical heat treatment furnace and the like. The carbon felt is typically prepared by pre-oxidizing and carbonizing an organic precursor.
Most carbon felts are prepared from Polyacrylonitrile (PAN) precursors. The Chinese patent CN113715425A prepares the carbon felt by taking polyacrylonitrile as a precursor, takes the polyacrylonitrile as a base material layer, prepares a light environment-friendly smokeless household electrical appliance heat insulation material through a series of processes of pressing, cutting and the like, but the prepared carbon felt is a soft felt, the heat insulation effect of the heat insulation layer is uneven, the temperature is uneven and unstable, the soft felt is easy to embrittle at high temperature, slag is removed, and the hearth and the environment are polluted. Chinese patent CN112980283a uses carbon felt as a base material, and prepares a surface thermal insulation coating on the surface of the carbon felt by compounding cellulose, resin, carbonized material and felt powder, and the thermal insulation performance needs to be further improved. Chinese patent CN113026349a uses polyacrylonitrile as a precursor, and a series of processes such as pre-oxidation, carbonization, graphitization, surface treatment, and outer surface treatment are performed to prepare a thermal insulation carbon felt, which is a hard felt, and compared with a soft felt, the mechanical strength of the carbon felt is improved, and the thermal insulation effect of the carbon felt is improved. However, the polyacrylonitrile is used as a precursor to prepare the non-woven felt, the needle breakage is particularly easy during the needle punching, and the prepared carbon felt is fragile and has poor mechanical properties, and the tensile strength of the carbon felt is not more than 100MPa. The non-woven felt prepared by taking the viscose-based fiber as a precursor has the advantages of tensile strength of more than 200MPa, low thermal conductivity as low as 0.05W/m.k, low graphitization degree, low modulus, 1% of elongation at break and good biocompatibility, however, the coarse denier viscose-based fiber has poor heat insulation performance.
Therefore, the viscose-based carbon fiber hard felt with good heat insulation performance, uniform heat insulation and excellent mechanical property is obtained by research, and has important value and significance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an ultrafine viscose-based carbon fiber heat insulation hard felt and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of an ultrafine viscose carbon fiber heat-insulating hard felt, which comprises the following steps:
1) Performing needling treatment on the superfine viscose fibers to obtain superfine viscose-based fiber mats;
2) Sequentially centrifuging and drying the superfine viscose-based fiber felt after being immersed in a catalyst system, and pre-oxidizing the dried product to obtain a pre-oxidized superfine viscose-based fiber felt;
3) And (3) immersing the pre-oxidized superfine viscose-based fiber felt in a phenolic resin solution, curing, and carbonizing a cured product to obtain the superfine viscose-based carbon fiber heat-insulating hard felt.
Preferably, the denier of the superfine viscose fiber in the step 1) is 0.45-0.6 dtex, and the gram weight of the superfine viscose-based fiber felt is 200-1200 g/m 2 。
Preferably, the catalyst system in the step 2) is an aqueous solution of acid and urea, wherein the total mass fraction of the acid and the urea in the catalyst system is 10-30%, and the mass ratio of the acid to the urea is 1:1-3; the acid is nitric acid or boric acid.
Preferably, the time of the dipping treatment in the step 2) is 10-40 min; the centrifugation time is 2-6 min, and the centrifugation speed is 2000-6000 r/min; the drying temperature is 70-90 ℃ and the drying time is 30-40 min.
Preferably, the pre-oxidation treatment in the step 2) is to perform pre-oxidation treatment on the dried product at 130-140 ℃, 165-175 ℃, 268-273 ℃, 278-282 ℃ and 283-287 ℃ in sequence to obtain a pre-oxidized superfine viscose-based fiber felt;
the pre-oxidation treatment time is 8-12 min at 130-140 ℃, the pre-oxidation treatment time is 12-18 min at 165-175 ℃, the pre-oxidation treatment time is 15-25 min at 268-273 ℃, the pre-oxidation treatment time is 15-25 min at 278-282 ℃ and the pre-oxidation treatment time is 22-28 min at 283-287 ℃;
the pre-oxidation treatment atmosphere is air atmosphere, and the pressure is 0.1-0.2 MPa.
Preferably, in the step 3), the mass concentration of the phenolic resin solution is 15-50%, and the solvent of the phenolic resin solution is ethanol;
the time of the dipping treatment is 25-35 min; the curing temperature is 160-180 ℃ and the curing time is 25-35 min.
Preferably, the carbonization atmosphere is a nitrogen atmosphere, and the pressure is 0.1-0.2 MPa;
the specific process of carbonization is that the solidified product is carbonized at 240-260 ℃, 290-310 ℃, 490-510 ℃ and 1300-1500 ℃ in sequence to obtain the superfine viscose carbon fiber heat insulation hard felt;
the carbonization time is 3-7 min at 240-260 ℃, 12-18 min at 290-310 ℃, 8-12 min at 490-510 ℃ and 8-12 min at 1300-1500 ℃.
Preferably, the impregnating treatment, curing and carbonization in the step 3) are repeatedly and alternately performed; the number of repeated alternation is 3 to 6.
The invention also provides the superfine viscose-based carbon fiber heat insulation hard felt prepared by the preparation method, wherein the heat conductivity of the superfine viscose-based carbon fiber heat insulation hard felt is 0.03-0.18W/m.k, and the tensile strength is 800-1050 MPa.
The beneficial effects of the invention include:
1) The invention adopts superfine viscose fiber as raw material, and obtains superfine viscose base fiber felt through needling, then prepares soft felt with high carbon yield through composite catalyst impregnation catalysis, and obtains superfine viscose base carbon fiber hard felt through multiple liquid phase impregnation, solidification and carbonization, and pyrolytic carbon formed after carbonization generates good adhesiveness with the pore wall inside the material, thereby improving the mechanical strength and heat insulation performance of the carbon felt.
2) The superfine viscose-based carbon fiber heat-insulating hard felt can solve the problems of poor heat-insulating performance of coarse denier viscose-based fibers and poor mechanical performance of common soft felts, effectively improves the heat-insulating performance of the carbon felts, prolongs the service life, can be applied to the field of heat insulation protection, and improves the mechanical performance of the carbon felts after phenolic resin impregnation treatment. The thermal conductivity of the superfine viscose carbon fiber hard felt is 0.03-0.18W/m.k, and the tensile strength is 800-1050 MPa.
Drawings
FIG. 1 is a physical diagram of an ultrafine viscose-based carbon fiber thermal insulation hard felt prepared in example 1;
FIG. 2 is an SEM image of an ultra-fine viscose-based carbon fiber thermal insulation hard felt prepared in example 1;
FIG. 3 is a Raman plot of the ultra-fine viscose-based carbon fiber insulation hard mat prepared in example 1;
fig. 4 is an XRD curve of the ultra fine viscose-based carbon fiber thermal insulation hard felt prepared in example 1.
Detailed Description
The invention provides a preparation method of an ultrafine viscose carbon fiber heat-insulating hard felt, which comprises the following steps:
1) Performing needling treatment on the superfine viscose fibers to obtain superfine viscose-based fiber mats;
2) Sequentially centrifuging and drying the superfine viscose-based fiber felt after being immersed in a catalyst system, and pre-oxidizing the dried product to obtain a pre-oxidized superfine viscose-based fiber felt;
3) And (3) immersing the pre-oxidized superfine viscose-based fiber felt in a phenolic resin solution, curing, and carbonizing a cured product to obtain the superfine viscose-based carbon fiber heat-insulating hard felt.
The denier of the superfine viscose fiber in the step 1) is preferably 0.45-0.6 dtex, more preferably 0.5-0.55 dtex, and the gram weight of the superfine viscose-based fiber felt is preferably 200-1200 g/m 2 Further preferably 300 to 1000g/m 2 More preferably 500 to 800g/m 2 。
The invention takes superfine viscose fiber as raw material, the superfine viscose fiber is spread on the panel of a carding machine, flattened, aligned, reciprocated for 2 times on the carding machine, spread the carded fiber on the feeding panel of a needling machine, and pre-needled for 1-3 times under a smaller needling strength, thus forming a needled non-woven material with certain thickness and certain strength. And then the needling intensity is increased to carry out main needling, so that the fabric is more compact, the felt is thinner, and the superfine viscose-based fiber felt is prepared by 2 back and forth steps on a needling machine.
The fine denier viscose-based fiber has good drapability, softness and drift feel, provides reliable guarantee for improving spun yarn strength and uniformity, can also reduce the thermal conductivity of the material, and remarkably improves the heat insulation performance of the material, so that the fine denier viscose-based fiber is more suitable for being used as a precursor for preparing a carbon felt.
The catalyst system in step 2) of the present invention is preferably an aqueous solution of an acid and urea, and the total mass fraction of the acid and urea in the catalyst system is preferably 10 to 30%, more preferably 15 to 25%, still more preferably 18 to 22%; the mass ratio of the acid to the urea is preferably 1:1-3, more preferably 1:2, and the acid is preferably nitric acid or boric acid; the mass concentration of nitric acid is preferably 65 to 68%, more preferably 66 to 67%.
The time of the dipping treatment in the step 2) is preferably 10 to 40min, more preferably 15 to 35min, and even more preferably 20 to 30min; the time of centrifugation is preferably 2 to 6 minutes, more preferably 3 to 5 minutes, and still more preferably 4 minutes; the rate of centrifugation is preferably 2000 to 6000r/min, more preferably 2500 to 5000r/min, still more preferably 3000 to 4500r/min; the drying temperature is preferably 70 to 90 ℃, more preferably 75 to 85 ℃, and even more preferably 80 ℃; the drying time is preferably 30 to 40 minutes, more preferably 32 to 38 minutes, and still more preferably 34 to 36 minutes.
The pre-oxidation treatment according to step 2) of the present invention is preferably carried out in a tube furnace.
The pre-oxidation treatment in the step 2) is preferably to pre-oxidize the dried product at 130-140 ℃, 165-175 ℃, 268-273 ℃, 278-282 ℃ 283-287 ℃ in sequence to obtain a pre-oxidized superfine viscose-based fiber felt, and more preferably to pre-oxidize the dried product at 135 ℃, 170 ℃, 270 ℃, 280 ℃ and 285 ℃ in sequence;
the time of the pre-oxidation treatment at 130 to 140 ℃ is preferably 8 to 12 minutes, more preferably 10 minutes; the time of the pre-oxidation treatment at 165-175 ℃ is preferably 12-18 min, more preferably 15min; the time of the pre-oxidation treatment at 268-273 ℃ is preferably 15-25 min, more preferably 20min; the time of the pre-oxidation treatment at 278-282 ℃ is preferably 15-25 min, more preferably 20min; the time for the pre-oxidation treatment at 283 to 287℃is preferably 22 to 28 minutes, more preferably 25 minutes.
In the pre-oxidation treatment of the invention, the heating rate from 50 ℃ to 130-140 ℃ is preferably 1-3 ℃/min, and more preferably 2 ℃/min; the heating rate from 130-140 ℃ to 165-175 ℃ is preferably 2-5 ℃/min, more preferably 3-4 ℃/min; the heating rate from 165-175 ℃ to 268-273 ℃ is preferably 3-8 ℃/min, more preferably 5-6 ℃/min; the heating rate from 268-273 ℃ to 278-282 ℃ is preferably 7-13 ℃/min, more preferably 10-11 ℃/min; the heating rate from 278 to 282 ℃ to 283 to 287 ℃ is preferably 7 to 13 ℃/min, more preferably 10 to 11 ℃/min;
the pre-oxidation treatment atmosphere in the present invention is preferably an air atmosphere, and the pressure is preferably 0.1 to 0.2MPa, and more preferably 0.15MPa.
The pre-oxidation treatment in the step 2) is completed, and deionized water is preferably used for washing 5-6 times after the tubular furnace is cooled to room temperature, and then the pretreated superfine viscose-based fiber felt is obtained after drying at 60 ℃.
The mass concentration of the phenolic resin solution in the step 3) is preferably 15-50%, more preferably 20-40%, and even more preferably 25-30%; the solvent of the phenolic resin solution is preferably absolute ethanol.
The time of the dipping treatment in the step 3) is preferably 25 to 35min, more preferably 27 to 32min, and even more preferably 30min; the curing temperature is preferably 160 to 180 ℃, more preferably 165 to 175 ℃, and even more preferably 170 ℃; the curing time is preferably 25 to 35 minutes, more preferably 27 to 32 minutes, and still more preferably 30 minutes; the curing is preferably carried out in a drying oven.
The atmosphere for carbonization in the present invention is preferably a nitrogen atmosphere, and the pressure is preferably 0.1 to 0.2MPa, and more preferably 0.15MPa.
The specific process of carbonization is that the cured product is carbonized at 240-260 ℃, 290-310 ℃, 490-510 ℃ and 1300-1500 ℃ in sequence to obtain the superfine viscose carbon fiber heat insulation hard felt, and the cured product is carbonized at 250-252 ℃, 295-300 ℃, 495-500 ℃ and 1350-1450 ℃ in sequence.
In the carbonization process, the carbonization time is preferably 3-7 min, more preferably 4-5 min at 240-260 ℃; the carbonization time at 290-310 ℃ is preferably 12-18 min, more preferably 15-16 min; the carbonization time at 490-510 ℃ is preferably 8-12 min, more preferably 15-16 min; the carbonization time at 1300 to 1500 ℃ is preferably 8 to 12 minutes, more preferably 10 to 11 minutes.
In the carbonization process, the temperature is increased from 50 ℃ to 240-260 ℃, from 240-260 ℃ to 290-310 ℃, from 290-310 ℃ to 490-510 ℃, and from 490-510 ℃ to 1300-1500 ℃, and the temperature increasing rate is independently preferably 8-12 ℃/min, and more preferably 10 ℃/min.
The dipping treatment, curing and carbonization are repeatedly and alternately carried out in the step 3); the number of repeating the alternation is preferably 3 to 6 times, more preferably 4 to 5 times.
The invention also provides the superfine viscose-based carbon fiber heat insulation hard felt prepared by the preparation method, wherein the heat conductivity of the superfine viscose-based carbon fiber heat insulation hard felt is preferably 0.03-0.18W/m.k, more preferably 0.05-0.12W/m.k, and the tensile strength is preferably 800-1050 MPa, more preferably 850-1000 MPa.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
30g of 0.45dtex superfine viscose fiber precursor yarn is spread on a carding machine panel, flattened, aligned and reciprocated on the carding machine for 2 times. Spreading the carded raw silk on a feeding panel of a needling machine, feeding the carded raw silk into the needling machine, pre-needling for 2 times, and then performing main needling to make the fabric more compact, make the felt thinner, and reciprocating for 2 times on the needling machine to obtain the productSuperfine viscose fiber felt (gram weight 500 g/m) 2 )。
Decocting superfine viscose-based fiber felt in boiling water for 10min to remove the treating agent on the surface of the fiber, taking out, putting into a baking oven, and drying at 60 ℃ for 12h. And then the dried superfine viscose-based fiber felt is completely immersed in an aqueous solution with the mass ratio of boric acid to urea being 1:2 (the total mass fraction of the boric acid and the urea in the aqueous solution is 20%) at room temperature, and is subjected to dipping treatment for 20 minutes. After the impregnation is completed, the mixture is placed into a self-made centrifuge tube, centrifuged for 4min at a speed of 3000r/min in a centrifuge, and then placed into an oven for drying at 80 ℃ for 35min.
Fixing the dried superfine viscose-based fiber felt by a graphite plate, placing the graphite plate into a tubular furnace for pre-oxidation treatment, wherein the pre-oxidation treatment is carried out under the air atmosphere and 0.15MPa, the temperature is raised to 135 ℃ from 50 ℃ at 2 ℃/min, the temperature is kept for 10min, the temperature is raised to 170 ℃ from 135 ℃ at 3 ℃/min, the temperature is kept for 15min, the temperature is raised to 270 ℃ from 5 ℃/min, the temperature is kept for 20min, the temperature is raised to 280 ℃ from 270 ℃ at 10 ℃/min, the temperature is kept for 20min, and the temperature is kept for 25min from 280 ℃ at 10 ℃/min. And after the tube furnace is cooled to room temperature, taking out the pre-oxidized fiber felt, washing the pre-oxidized fiber felt with deionized water for 6 times, and drying the pre-oxidized fiber felt at 60 ℃ for 12 hours to obtain the pre-oxidized superfine viscose-based fiber felt.
Uniformly mixing 20g of phenolic resin and 30g of absolute ethyl alcohol, completely immersing the pre-oxidized superfine viscose-based fiber felt in the phenolic resin ethanol solution, carrying out immersion treatment for 30min, and then curing for 30min in a drying oven at 170 ℃. Fixing the solidified fiber mat by using a graphite plate, placing the fiber mat into a tube furnace for carbonization treatment, wherein the carbonization treatment is carried out under the nitrogen atmosphere and 0.15MPa, and the specific steps are that the temperature is raised to 250 ℃ from 50 ℃ at 10 ℃/min, the temperature is kept for 5min, the temperature is raised to 300 ℃ from 250 ℃ at 10 ℃/min, the temperature is kept for 15min, the temperature is raised to 500 ℃ from 300 ℃ at 10 ℃/min, the temperature is kept for 10min, and the temperature is finally raised to 1400 ℃ from 500 ℃ at 10 ℃/min, and the temperature is kept for 10min. And (3) after the tubular furnace is cooled to room temperature, taking out the carbonized fiber felt, immersing the fiber felt in a phenolic resin ethanol solution, solidifying and carbonizing (the technological parameters are the same as those of the first time), carrying out immersing, solidifying and carbonizing in the phenolic resin ethanol solution, carrying out total circulation for 4 times, washing with deionized water for 6 times, and drying at 60 ℃ for 12 hours to obtain the superfine viscose-based carbon fiber heat-insulating hard felt.
The pre-oxidized superfine viscose-based fiber felt before being immersed in the phenolic resin solution is a superfine viscose-based fiber soft felt, the pre-oxidation yield of the soft felt is 57.31%, and the carbon yield of the superfine viscose-based fiber soft felt is 33.6%; the thermal conductivity of the superfine viscose-based carbon fiber heat insulation hard felt of the embodiment is 0.0647W/m.k, the tensile strength is 1000MPa, and the carbonization rate of the superfine viscose-based fiber felt after carbonization is 93.67%.
The physical diagram of the superfine viscose-based carbon fiber thermal insulation hard felt prepared in the embodiment is shown in fig. 1, the SEM diagram of the superfine viscose-based carbon fiber thermal insulation hard felt is shown in fig. 2, the raman curve of the superfine viscose-based carbon fiber thermal insulation hard felt is shown in fig. 3, and the XRD curve of the superfine viscose-based carbon fiber thermal insulation hard felt is shown in fig. 4. As can be seen from fig. 1 and 2, the phenolic resin particles are uniformly coated on the surface of the superfine viscose-based carbon fiber, which indicates that the phenolic resin is well immersed into the carbon felt; as can be seen from FIG. 3, at 1348cm -1 And 1591cm -1 Obvious characteristic diffraction peaks appear at the nearby positions, and the ID/IG is 0.99, which indicates that the graphitization degree of the superfine viscose-based carbon fiber heat-insulating hard felt is higher, and the oxidation resistance, the heat conductivity and the chemical stability of the superfine viscose-based carbon fiber heat-insulating hard felt are further improved; as can be seen from FIG. 4, the graphite crystals in the ultra-fine viscose-based carbon fiber thermal insulation hard felt have good orientation degree along the axial direction, which indicates that the graphitization degree is high, and the oxidation resistance, the thermal conductivity and the chemical stability of the ultra-fine viscose-based carbon fiber thermal insulation hard felt are further improved.
Example 2
Except that the phenolic resin of example 1 was changed to 10g of phenolic resin and 40g of absolute ethanol, and the conditions were the same as in example 1.
The pre-oxidized superfine viscose-based fiber felt before being immersed in the phenolic resin solution is a superfine viscose-based fiber soft felt, and the carbon yield of the superfine viscose-based fiber soft felt is 33.6%; the thermal conductivity of the superfine viscose-based carbon fiber heat insulation hard felt of the embodiment is 0.0647W/m.k, and the tensile strength is 1000MPa.
Example 3
The same conditions as in example 1 were applied, except that the total cycle of the impregnation treatment, curing and carbonization treatment in the phenolic resin ethanol solution was carried out 3 times, with the phenolic resin 20g and the absolute ethanol 30g of example 1 being changed to the phenolic resin 15g and the absolute ethanol 35 g.
The pre-oxidized superfine viscose-based fiber felt before being immersed in the phenolic resin solution is a superfine viscose-based fiber soft felt, and the carbon yield of the superfine viscose-based fiber soft felt is 31.3%; the thermal conductivity of the superfine viscose-based carbon fiber heat insulation hard felt of the embodiment is 0.1249W/m.k, and the tensile strength is 939MPa.
Example 4
The boric acid is changed to nitric acid on the basis of the embodiment 1, the mass ratio of the nitric acid to the urea is changed to 1:3, the total mass fraction of the nitric acid and the urea in the aqueous solution is changed to 30%, and the concentration of the nitric acid is 66%; the mass of the phenolic resin and the mass of the absolute ethyl alcohol were changed to 10g and 40g, respectively, and the total cycle of the impregnation treatment, the curing treatment and the carbonization treatment was carried out 3 times in the phenolic resin ethanol solution, and the other conditions were the same as in example 1.
The pre-oxidized superfine viscose-based fiber felt before being immersed in the phenolic resin solution is a superfine viscose-based fiber soft felt, and the carbon yield of the superfine viscose-based fiber soft felt is 35.5%; the thermal conductivity of the superfine viscose-based carbon fiber heat insulation hard felt of the embodiment is 0.0923W/m.k, and the tensile strength is 938MPa.
Example 5
Boric acid is changed to nitric acid on the basis of the embodiment 1, the mass ratio of nitric acid to urea is changed to 1:3, the total mass fraction of nitric acid and urea in aqueous solution is changed to 30%, and the concentration of nitric acid is 67%; the mass of the phenolic resin and the absolute ethanol were changed to 15g and 35g, respectively, and the other conditions were the same as in example 1.
The pre-oxidized superfine viscose-based fiber felt before being immersed in the phenolic resin solution is a superfine viscose-based fiber soft felt, and the carbon yield of the superfine viscose-based fiber soft felt is 33.3%; the thermal conductivity of the superfine viscose-based carbon fiber heat insulation hard felt of the embodiment is 0.1466W/m.k, and the tensile strength is 987MPa.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (7)
1. The preparation method of the superfine viscose-based carbon fiber heat insulation hard felt is characterized by comprising the following steps of:
1) Performing needling treatment on the superfine viscose fibers to obtain superfine viscose-based fiber mats;
2) Sequentially centrifuging and drying the superfine viscose-based fiber felt after being immersed in a catalyst system, and pre-oxidizing the dried product to obtain a pre-oxidized superfine viscose-based fiber felt;
3) The pre-oxidized superfine viscose-based fiber felt is cured after being immersed in a phenolic resin solution, and a cured product is carbonized to obtain the superfine viscose-based carbon fiber heat insulation hard felt;
the mass concentration of the phenolic resin solution in the step 3) is 15-50%, and the solvent of the phenolic resin solution is ethanol;
the time of the dipping treatment is 25-35 min; the curing temperature is 160-180 ℃ and the curing time is 25-35 min;
the carbonization atmosphere is nitrogen atmosphere, and the pressure is 0.1-0.2 MPa;
the specific process of carbonization is that the solidified product is carbonized at 240-260 ℃, 290-310 ℃, 490-510 ℃ and 1300-1500 ℃ in sequence to obtain the superfine viscose carbon fiber heat insulation hard felt;
the carbonization time is 3-7 min at 240-260 ℃, 12-18 min at 290-310 ℃, 8-12 min at 490-510 ℃ and 8-12 min at 1300-1500 ℃.
2. The method according to claim 1, wherein the superfine viscose fiber in step 1) has a denier of 0.45-0.6 dtex and a gram weight of 200-1200 g/m 2 。
3. The preparation method according to claim 1 or 2, wherein the catalyst system in step 2) is an aqueous solution of acid and urea, and the total mass fraction of the acid and urea in the catalyst system is 10-30%, and the mass ratio of the acid to the urea is 1:1-3; the acid is nitric acid or boric acid.
4. The method according to claim 3, wherein the time of the dipping treatment in step 2) is 10 to 40 minutes; the centrifugation time is 2-6 min, and the centrifugation speed is 2000-6000 r/min; the drying temperature is 70-90 ℃ and the drying time is 30-40 min.
5. The method according to claim 4, wherein the pre-oxidizing treatment in step 2) is to perform pre-oxidizing treatment on the dried product at 130-140 ℃, 165-175 ℃, 268-273 ℃, 278-282 ℃ and 283-287 ℃ in sequence to obtain a pre-oxidized superfine viscose-based fiber mat;
the pre-oxidation treatment time is 8-12 min at 130-140 ℃, the pre-oxidation treatment time is 12-18 min at 165-175 ℃, the pre-oxidation treatment time is 15-25 min at 268-273 ℃, the pre-oxidation treatment time is 15-25 min at 278-282 ℃ and the pre-oxidation treatment time is 22-28 min at 283-287 ℃;
the pre-oxidation treatment atmosphere is air atmosphere, and the pressure is 0.1-0.2 MPa.
6. The method according to claim 5, wherein the impregnating treatment, curing, and carbonization in step 3) are repeatedly and alternately performed; the number of repeated alternation is 3 to 6.
7. The superfine viscose-based carbon fiber heat insulation hard felt prepared by the preparation method of any one of claims 1 to 6 is characterized in that the thermal conductivity of the superfine viscose-based carbon fiber heat insulation hard felt is 0.03 to 0.18W/m.k, and the tensile strength is 800 to 1050MPa.
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