CN109576899A - A kind of environment-friendly solidified carbon felt and preparation method thereof - Google Patents
A kind of environment-friendly solidified carbon felt and preparation method thereof Download PDFInfo
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- CN109576899A CN109576899A CN201910038622.6A CN201910038622A CN109576899A CN 109576899 A CN109576899 A CN 109576899A CN 201910038622 A CN201910038622 A CN 201910038622A CN 109576899 A CN109576899 A CN 109576899A
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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
- D04H1/4266—Natural fibres not provided for in group D04H1/425
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01C—CHEMICAL OR BIOLOGICAL TREATMENT OF NATURAL FILAMENTARY OR FIBROUS MATERIAL TO OBTAIN FILAMENTS OR FIBRES FOR SPINNING; CARBONISING RAGS TO RECOVER ANIMAL FIBRES
- D01C1/00—Treatment of vegetable material
- D01C1/02—Treatment of vegetable material by chemical methods to obtain bast fibres
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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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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B9/00—Solvent-treatment of textile materials
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- D—TEXTILES; PAPER
- 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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Abstract
The present invention discloses a kind of environment-friendly solidified carbon felt and preparation method thereof, and the solidification carbon felt is prepared by raw material of natural bamboo fibres；The preparation method for solidifying carbon felt includes: to cut and degumming, pickling and throwing, acid processing and softening, shredding and felt, carbonization and sizing, CVD processing and high-temperature process.Compared with existing solidification carbon felt preparation method, solidification carbon felt preparation method environmental protection provided by the invention, and raw material sources are abundant, cheap；The filament diameter provided by the invention for solidifying carbon felt is 10~15 μm；The solidification carbon felt is mainly carbon, and carbon element content is 95~97%；The solidification carbon felt highest is resistant to 2500 DEG C, and metals content impurity is lower than 295ppm.
Description
Technical field
The present invention relates to thermal insulation material preparation technical field, especially a kind of environment-friendly solidified carbon felt and preparation method thereof.
Background technique
Ingot furnace, single crystal growing furnace, the main parts size for hydrogenating furnace thermal field system are manufactured, required heat-insulation and heat-preservation solidifies felt,
The excellent properties such as high temperature resistant are needed, also require metals content impurity lower than 300ppm, are just able to satisfy artificial lens Cheng Jing and higher
The requirement of yield rate.
Traditional artificial crystal growth furnace heat-insulation and heat-preservation component uses graphite and soft carbon felt component.
Since last century end, it is thus proposed that manufacture thermal field part with carbon-carbon composite.Existing most manufacture thermal field
In the method for part, the raw material that manufacture solidifies carbon felt are all made of PAN (polyacrylonitrile) carbon fiber or PAN carbon fiber felt, PAN
Carbon fiber be by petroleum product propylene by polymerization, nitrilation, reeling off raw silk from cocoons is made precursor, precursor process pre-oxidation, low-temperature carbonization, high temperature
Made of carbonization, energy consumption is high for preparation process, and environmental pollution is big, and manufacturing technology requires height, and the manufacturing cycle is long, expensive.
It is environmentally friendly there are also the method for solidifying carbon felt using natural ramie fiber manufacture in the method for existing manufacture thermal field part,
Raw material sources are abundant, cheap.But it proposes higher requirement to the raw material of flaxen fiber, need to select available phosphorus content
The fibre of flax for textile material of soil plantation less than 15mg/kg is used as flaxen fiber raw material, and the raw material are rare and difficult searching, price compared with
It is high.
Summary of the invention
The present invention provides a kind of environment-friendly solidified carbon felt and preparation method thereof, and for overcoming, energy consumption is high in the prior art, environment
The defects of pollution is big and the prices of raw materials are high and hardly possible obtains, realizes preparation method environmental protection, and raw material sources are abundant, price is low
It is honest and clean.
To achieve the above object, the present invention proposes that a kind of environment-friendly solidified carbon felt, the solidification carbon felt are with natural bamboo fibres
Raw material；The filament diameter for solidifying carbon felt is 10~15 μm；The solidification carbon felt is mainly carbon, and carbon element content is
95~97%；The solidification carbon felt highest is resistant to 2500 DEG C, and metals content impurity is lower than 295ppm.
To achieve the above object, the present invention also proposes a kind of preparation method of environment-friendly solidified carbon felt, comprising the following steps:
S1: bamboo is cut into bamboo cane, the bamboo cane is put into degumming agent impregnates degumming later, use deionized water later
It rinses；
S2: by step S1, treated that bamboo cane is impregnated in concentrated hydrochloric acid, is rinsed later with deionized water, later by institute
It states bamboo cane and carries out throwing with hydraulic press, obtain bamboo silk；
S3: the silk of bamboo obtained by step S2 is put into reactive tank, and dilute hydrochloric acid is added, and heating is pressurizeed, later heat-insulation pressure keeping；It will
Acid treated bamboo silk is rinsed with deionized water, and is carried out dehydrating with centrifuge；
S4: the silk of bamboo obtained by step S3 is put into softening agent and carries out softening immersion treatment；Then bamboo silk is put into baking oven
Drying；
S5: step S4 treated bamboo silk is put into scutching fluffer and carries out clear bullet, obtains sheet bamboo wadding, later shredding 1~3
It is secondary；Bamboo is wadded a quilt with cotton lapping later, is pierced through needing machine needle into bamboo felt；
S6: by step S5 treated bamboo felt is put into nitrogen protection furnace progress medium temperature carbonization treatment；Later by medium temperature carbon
Curing agent after changing treated, bamboo felt body uniformly penetrating into dilution, the heat preservation solidification sizing in curing oven；Bamboo felt is sent into later
High temperature cabonization is carried out in carburizing reagent furnace, obtains bamboo carbon felt；
S7: bamboo carbon felt obtained by step S6 is subjected to CVD processing；
S8: by step S7, treated that bamboo carbon felt is put into high temperature furnace carries out high-temperature process, obtains the solidification carbon felt.
Compared with prior art, the beneficial effects of the present invention are as follows:
1, the filament diameter provided by the invention for solidifying carbon felt is 10~15 μm, and predominantly carbon, carbon element content is
95~97%；The solidification carbon felt highest is resistant to 2500 DEG C, and metals content impurity is lower than 295ppm (mg/L), and can satisfy makes
Use demand.
2, the preparation method provided by the invention for solidifying carbon felt, using natural bamboo fibres as raw material, with use PAN carbon fiber
It is compared for raw material, it is more environmentally friendly, and reduce cost；With using flaxen fiber, raw material sources are richer compared with raw material.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
The structure shown according to these attached drawings obtains other attached drawings.
Fig. 1 is curing method flow chart of the present invention；
Fig. 2 is that hollow cylindrical solidification carbon felt expanded view is prepared in embodiment one.
Drawing reference numeral explanation: 1: bamboo carbon fibre.
The embodiments will be further described with reference to the accompanying drawings for the realization, the function and the advantages of the object of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiment is only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts it is all its
His embodiment, shall fall within the protection scope of the present invention.
It is to be appreciated that the directional instruction (such as up, down, left, right, before and after ...) of institute is only used in the embodiment of the present invention
In explaining in relative positional relationship, the motion conditions etc. under a certain particular pose (as shown in the picture) between each component, if should
When particular pose changes, then directionality instruction also correspondingly changes correspondingly.
In addition, the description for being such as related to " first ", " second " in the present invention is used for description purposes only, and should not be understood as
Its relative importance of indication or suggestion or the quantity for implicitly indicating indicated technical characteristic.Define as a result, " first ",
The feature of " second " can explicitly or implicitly include at least one of the features.In the description of the present invention, " multiple " contain
Justice is at least two, such as two, three etc., unless otherwise specifically defined.
In the present invention unless specifically defined or limited otherwise, term " connection ", " fixation " etc. shall be understood in a broad sense,
For example, " fixation " may be a fixed connection, it may be a detachable connection, or integral；It can be mechanical connection, be also possible to
Electrical connection can also be physical connection or wireless communication connection；It can be directly connected, the indirect phase of intermediary can also be passed through
Even, the connection inside two elements or the interaction relationship of two elements be can be, unless otherwise restricted clearly.For this
For the those of ordinary skill in field, the specific meanings of the above terms in the present invention can be understood according to specific conditions.
It in addition, the technical solution between each embodiment of the present invention can be combined with each other, but must be general with this field
Based on logical technical staff can be realized, it will be understood that when the combination of technical solution appearance is conflicting or cannot achieve this
The combination of technical solution is not present, also not the present invention claims protection scope within.
The present invention proposes a kind of environment-friendly solidified carbon felt, and the solidification carbon felt is using natural bamboo fibres as raw material；The solidification
The filament diameter of carbon felt is 10~15 μm；The solidification carbon felt is mainly carbon, and carbon element content is 95~97%；It is described solid
Change carbon felt highest and be resistant to 2500 DEG C, metals content impurity is lower than 295ppm.
The present invention also proposes a kind of preparation method (referring to Fig.1) of environment-friendly solidified carbon felt, comprising the following steps:
S1: cutting and degumming, bamboo is cut into the bamboo cane of long 500~1500mm, wide 10~20mm, later by the bamboo
Item, which is put into degumming agent, impregnates degumming, is rinsed well later with deionized water；Cut is in order to better degumming；Degumming process
It is to slough the pectin in bamboo fibre, adipocere matter etc..
S2: pickling and throwing, by step S1, treated that bamboo cane is impregnated in concentrated hydrochloric acid, is rushed later with deionized water
The bamboo cane is carried out throwing with hydraulic press later by wash clean, obtains bamboo silk；The pickling is to remove the gold in bamboo fibre
Belong to element and inorganic elements, such as K, Na, S, P.
S3: the silk of bamboo obtained by step S2 is put into reactive tank by acid processing, and dilute hydrochloric acid is added, and heating, pressurization are kept the temperature later
Pressure maintaining；Acid treated bamboo silk is rinsed with deionized water, and is carried out dehydrating with centrifuge；Acid processing is further gone
Except metallic element remaining in bamboo fibre and inorganic elements.
S4: the silk of bamboo obtained by step S3 is put into softening agent and carries out softening immersion treatment by softening；Then bamboo silk is put into baking
It is dried in case；Softening is for the ease of shredding later, and the sheet bamboo wadding for obtaining shredding is soft, is convenient for felt.
S5: shredding and felt, by step S4, treated that bamboo silk is put into scutching fluffer carries out clear bullet, obtains sheet bamboo wadding,
Shredding later 1~3 time；Bamboo is wadded a quilt with cotton lapping later, is pierced through needing machine needle into bamboo felt.
S6: by step S5 treated bamboo felt is put into nitrogen protection furnace progress medium temperature carbonization treatment；Later by medium temperature carbon
Curing agent after changing treated, bamboo felt body uniformly penetrating into dilution, the heat preservation solidification sizing in curing oven；Bamboo felt is sent into later
High temperature cabonization is carried out in carburizing reagent furnace, obtains bamboo carbon felt；
Carbonization treatment is while to remove the impurity in molecule to make bamboo fibre inorganic molecule be carbonized, and it is fine to improve bamboo
Carbon content in dimension.Sheet, tubular, taper etc. can be made in setting treatment as needed.Curing agent is first carried out with diluent
Dilution is appearance phenomena such as cracking in carbonisation in order to prevent.
Bamboo carbon felt obtained by step S6 is carried out CVD processing by S7:CVD processing；The CVD processing can increase in bamboo fibre
Carbon content, while continuity, rub resistance and the corrosion resistance etc. for improving bamboo fibre.
S8: high-temperature process, by step S7, treated that bamboo carbon felt is put into high temperature furnace carries out high-temperature process, obtains described solid
Change carbon felt.High-temperature process is the carbon content in order to further increase bamboo fibre, other impurities element is removed, so that finally obtained
The carbon content for solidifying carbon felt is 95~97%.
Preferably, in the step S1, the bamboo is diameter >=10cm bamboo；Selectable bamboo type includes:
Bamboo, the bamboo of the Ladies of the Xiang, mottled bamboo etc..Diameter >=10cm bamboo growth and maturity, bamboo fibre content is high, high-quality.
The degumming agent is NaHCO3、Na2CO3Or NaOH is one such, NaHCO3、Na2CO3Or the concentration 25% of NaOH
~45%, it is complete to be conducive to degumming, and do not influence its original performance.
The immersion degumming is at 90~110 DEG C, 3~5h of heat-insulation soaking, so that degumming is more abundant.
Preferably, in the step S2, the mass fraction of the concentrated hydrochloric acid is 20%-38%；It is described to impregnate in room temperature
20~40min of lower immersion.Under the preferred conditions be more conducive to removal bamboo fibre in metallic element and inorganic elements, as K, Na,
S, P etc..
Preferably, in the step S3, the mass fraction of the dilute hydrochloric acid is 10%~20%；The temperature of the heating and thermal insulation
Degree is 45~80 DEG C, the too high HCl highly volatile of temperature, and the too low impurity element removal rate of temperature is low；The pressure of the pressurization pressure maintaining
For 1.4~1.6MPa；The time of the heat-insulation pressure keeping is 5~8h.It is more conducive to remain in removal bamboo fibre under the preferred conditions
Metallic element and inorganic elements.
Preferably, in the step S4, the softening agent is one of sulfonated oil or silicone oil；It is described softening impregnate when
Between be 1~5h；The temperature of the drying is 200~260 DEG C, and the time is 4~6h.Flexibility can be obtained more under the preferred conditions
Good bamboo silk, in favor of subsequent shredding.
Preferably, in the step S5, dust and impurities will be shrugged off after each shredding, avoid bringing impurity member into
Element；The needle set of the shredding is made of bamboo stick, avoids bringing impurity element into.
Preferably, in the step S6, the temperature of the medium temperature carbonization treatment is 500 DEG C~800 DEG C, the time is 10~
20h；The curing agent includes colloid or resin；Diluent used by the dilution be alcohol or methanol, dilution ratio 1:
(6~8)；The temperature of the solidifying and setting is 150~250 DEG C, and the time is 5~10h；The temperature of the high temperature cabonization be 1100~
1400 DEG C, the time is 5~20h.Preferably, in the step S7, the temperature of CVD processing is 950~1050 DEG C, and the time is
10~20h, carbon-source gas are one of natural gas, methane or propane gas.
Preferably, in the step S8, the temperature of the high-temperature process is 2000~2500 DEG C, and the time is 5~10h.Temperature
Degree too low-carbon is incomplete, and the too high carbon felt of temperature does not tolerate.
Carbon element content: the Japanese infrared sulphur carbon analyzer of EMGA-820 type；
Metal impurities: Agilent-5110ICP-OES (inductive coupling plasma emission spectrograph).
Embodiment one
The present embodiment provides a kind of preparation methods of environment-friendly solidified carbon felt, comprising the following steps:
S1: cutting and degumming, and bamboo is cut into the bamboo cane of long 500mm, width 10mm, the bamboo cane is put into concentration later
For 25% NaHCO3In solution, heat-insulation soaking 3h, is rinsed well with deionized water later at 90 DEG C；
S2: pickling and throwing are impregnated in the concentrated hydrochloric acid for being 20% by step S1 treated bamboo cane is put into mass fraction
20min is rinsed well with deionized water later, and the bamboo cane is carried out throwing with hydraulic press later, obtains bamboo silk；
S3: the silk of bamboo obtained by step S2 is put into reactive tank by acid processing, is added in the dilute hydrochloric acid that mass fraction is 10%,
It is heated to 80 DEG C, is forced into 1.5MPa, later heat-insulation pressure keeping 5h under the conditions of 80 DEG C, 1.5MPa；Acid treated bamboo silk is used
Deionized water is rinsed, and is carried out dehydrating with centrifuge；
S4: the silk of bamboo obtained by step S3 is put into sulfonated oil and impregnates 1h by softening；Then bamboo silk is put into baking oven 200 DEG C
Dry 4h；
S5: shredding and felt, by step S4, treated that bamboo silk is put into scutching fluffer carries out clear bullet, obtains sheet bamboo wadding,
Shredding later 1 time；Bamboo is wadded a quilt with cotton lapping later, is pierced through needing machine needle into bamboo felt；
S6: carbonization and sizing, by step S5 treated bamboo felt is put into nitrogen protection furnace progress medium temperature carbonization treatment, institute
The temperature for stating medium temperature carbonization treatment is 500 DEG C, time 10h；The bamboo felt body after medium temperature carbonization treatment is uniformly penetrated into use later
The resin (dilution ratio 1:7) that alcohol diluted, 150 DEG C of heat preservation 5h solidifying and settings are hollow cylindrical in curing oven；Later
Bamboo felt is sent into carburizing reagent furnace and carries out high temperature cabonization, the temperature of the high temperature cabonization is 1100 DEG C, and time 5h obtains bamboo carbon
Felt；
Bamboo carbon felt obtained by step S6 is carried out CVD processing by S7:CVD processing；The temperature of the CVD processing is 950 DEG C, when
Between be 10h, carbon-source gas is natural gas.
S8: high-temperature process, by step S7, treated that bamboo carbon felt is put into high temperature furnace carries out high-temperature process, at the high temperature
The temperature of reason is 2000 DEG C, time 5h, obtains the solidification carbon felt (referring to Fig. 2).
The filament diameter of solidification carbon felt obtained by the present embodiment is 10 μm；The solidification carbon felt includes carbon and hydrogen member
Element, and carbon element content is up to 96.4%；The solidification carbon felt highest is resistant to 2500 DEG C, metals content impurity 287ppm.
Embodiment two
The present embodiment provides a kind of preparation methods of environment-friendly solidified carbon felt, comprising the following steps:
S1: cutting and degumming, and bamboo is cut into the bamboo cane of long 850mm, width 14mm, the bamboo cane is put into concentration later
For 30% Na2CO3In solution, heat-insulation soaking 3.5h, is rinsed well with deionized water later at 105 DEG C；
S2: pickling and throwing are impregnated in the concentrated hydrochloric acid for being 27% by step S1 treated bamboo cane is put into mass fraction
27min is rinsed well with deionized water later, and the bamboo cane is carried out throwing with hydraulic press later, obtains bamboo silk；
S3: the silk of bamboo obtained by step S2 is put into reactive tank by acid processing, is added in the dilute hydrochloric acid that mass fraction is 15%,
It is heated to 60 DEG C, is forced into 1.6MPa, later heat-insulation pressure keeping 6h under the conditions of 60 DEG C, 1.6MPa；Acid treated bamboo silk is used
Deionized water is rinsed, and is carried out dehydrating with centrifuge；
S4: the silk of bamboo obtained by step S3 is put into sulfonated oil and impregnates 2.5h by softening；Then bamboo silk is put into 220 in baking oven
DEG C dry 4.5h；
S5: shredding and felt, by step S4, treated that bamboo silk is put into scutching fluffer carries out clear bullet, obtains sheet bamboo wadding,
Shredding later 2 times；Bamboo is wadded a quilt with cotton lapping later, is pierced through needing machine needle into bamboo felt；
S6: carbonization and sizing, by step S5 treated bamboo felt is put into nitrogen protection furnace progress medium temperature carbonization treatment, institute
The temperature for stating medium temperature carbonization treatment is 650 DEG C, time 14h；The bamboo felt body after medium temperature carbonization treatment is uniformly penetrated into glue later
Body (dilution ratio 1:7), 180 DEG C of heat preservation 6.5h solidifying and settings are sheet in curing oven；Bamboo felt is sent into carburizing reagent later
High temperature cabonization is carried out in furnace, the temperature of the high temperature cabonization is 1200 DEG C, and time 9h obtains bamboo carbon felt；
Bamboo carbon felt obtained by step S6 is carried out CVD processing by S7:CVD processing；The temperature of the CVD processing is 1000 DEG C, when
Between be 14h, carbon-source gas is methane.
S8: high-temperature process, by step S7, treated that bamboo carbon felt is put into high temperature furnace carries out high-temperature process, at the high temperature
The temperature of reason is 2200 DEG C, time 7h, obtains the solidification carbon felt.
The filament diameter of solidification carbon felt obtained by the present embodiment is 12 μm；The solidification carbon felt includes carbon and hydrogen member
Element, and carbon element content is up to 96%；The solidification carbon felt highest is resistant to 2500 DEG C, metals content impurity 292ppm.
Embodiment three
The present embodiment provides a kind of preparation methods of environment-friendly solidified carbon felt, comprising the following steps:
S1: cutting and degumming, and bamboo is cut into the bamboo cane of long 1500mm, width 20mm, is later put into the bamboo cane dense
Degree is in 45% NaOH solution, heat-insulation soaking 5h, rinses later with deionized water at 110 DEG C well；
S2: pickling and throwing are impregnated in the concentrated hydrochloric acid for being 38% by step S1 treated bamboo cane is put into mass fraction
40min is rinsed well with deionized water later, and the bamboo cane is carried out throwing with hydraulic press later, obtains bamboo silk；
S3: the silk of bamboo obtained by step S2 is put into reactive tank by acid processing and softening, and dilute salt that mass fraction is 20% is added
It in acid, is heated to 45 DEG C, is forced into 1.4MPa, later heat-insulation pressure keeping 8h under the conditions of 100 DEG C, 1.4MPa；By acid, treated
Bamboo silk is rinsed with deionized water, and is carried out dehydrating with centrifuge；
S4: the silk of bamboo obtained by step S3 is put into silicone oil and impregnates 5h；Then bamboo silk is put into 260 DEG C of baking 6h in baking oven；
S5: shredding and felt, by step S4, treated that bamboo silk is put into scutching fluffer carries out clear bullet, obtains sheet bamboo wadding,
Shredding later 3 times；Bamboo is wadded a quilt with cotton lapping later, is pierced through needing machine needle into bamboo felt；
S6: carbonization and sizing, by step S5 treated bamboo felt is put into nitrogen protection furnace progress medium temperature carbonization treatment, institute
The temperature for stating medium temperature carbonization treatment is 800 DEG C, time 20h；The bamboo felt body after medium temperature carbonization treatment is uniformly penetrated into use later
Resin (dilution ratio 1:8) after methanol dilution, 250 DEG C of heat preservation 10h solidifying and settings are rodlike in curing oven；Later by bamboo felt
It is sent into carburizing reagent furnace and carries out high temperature cabonization, the temperature of the high temperature cabonization is 1400 DEG C, and time 20h obtains bamboo carbon felt；
Bamboo carbon felt obtained by step S6 is carried out CVD processing by S7:CVD processing；The temperature of the CVD processing is 1050 DEG C, when
Between be 20h, carbon-source gas is propane.
S8: high-temperature process, by step S7, treated that bamboo carbon felt is put into high temperature furnace carries out high-temperature process, at the high temperature
The temperature of reason is 2500 DEG C, time 10h, obtains the solidification carbon felt.
The filament diameter of solidification carbon felt obtained by the present embodiment is 15 μm；The solidification carbon felt includes carbon and hydrogen member
Element, and carbon element content is up to 95%；The solidification carbon felt highest is resistant to 2500 DEG C, metals content impurity 283ppm.
Example IV
The present embodiment provides a kind of preparation method of environment-friendly solidified carbon felt,
Compared with embodiment one, the present embodiment: S2: the mass fraction of concentrated hydrochloric acid is 37%, S3: the mass fraction of dilute hydrochloric acid
It is 18% other steps with embodiment one.
The filament diameter of solidification carbon felt obtained by the present embodiment is 11 μm；The solidification carbon felt includes carbon and hydrogen member
Element, and carbon element content is up to 97%；The solidification carbon felt highest is resistant to 2500 DEG C, metals content impurity 279ppm.
Embodiment five
The present embodiment provides a kind of preparation method of environment-friendly solidified carbon felt,
Compared with embodiment one, the present embodiment: S5: the temperature of the medium temperature carbonization treatment is 600 DEG C, time 10h；It
Afterwards by the bamboo felt body resin (dilution ratio 1:7) that uniformly infiltration was diluted with alcohol after medium temperature carbonization treatment, in curing oven
175 DEG C of heat preservation 5h solidifying and settings are hollow cylindrical；Bamboo felt is sent into carburizing reagent furnace later and carries out high temperature cabonization, the height
The temperature of temperature carbonization is 1150 DEG C, and time 5h obtains bamboo carbon felt；
Other steps are the same as embodiment one.
The filament diameter of solidification carbon felt obtained by the present embodiment is 10.5 μm；The solidification carbon felt includes carbon and hydrogen
Element, and carbon element content is up to 96.6%；The solidification carbon felt highest is resistant to 2500 DEG C, metals content impurity 285ppm.
The above description is only a preferred embodiment of the present invention, is not intended to limit the scope of the invention, all at this
Under the inventive concept of invention, using equivalent structure transformation made by description of the invention and accompanying drawing content, or directly/use indirectly
It is included in other related technical areas in scope of patent protection of the invention.
Claims (10)
1. a kind of environment-friendly solidified carbon felt, which is characterized in that the solidification carbon felt is using natural bamboo fibres as raw material；The solidification carbon
The filament diameter of felt is 10~15 μm；The solidification carbon felt is mainly carbon, and carbon element content is 95~97%；The solidification
Carbon felt highest is resistant to 2500 DEG C, and metals content impurity is lower than 295ppm.
2. a kind of preparation method of environment-friendly solidified carbon felt, which comprises the following steps:
S1: bamboo is cut into bamboo cane, the bamboo cane is put into degumming agent impregnates degumming later, rushed later with deionized water
It washes；
S2: by step S1, treated that bamboo cane is impregnated in concentrated hydrochloric acid, is rinsed later with deionized water, later by the bamboo
Item carries out throwing with hydraulic press, obtains bamboo silk；
S3: the silk of bamboo obtained by step S2 is put into reactive tank, and dilute hydrochloric acid is added, and heating is pressurizeed, later heat-insulation pressure keeping；At acid
Bamboo silk after reason is rinsed with deionized water, and is carried out dehydrating with centrifuge；
S4: the silk of bamboo obtained by step S3 is put into softening agent and carries out softening immersion treatment；Then bamboo silk is put into baking oven and is dried；
S5: step S4 treated bamboo silk being put into scutching fluffer and carries out clear bullet, obtains sheet bamboo wadding, and shredding later 1~3 time；
Bamboo is wadded a quilt with cotton lapping later, is pierced through needing machine needle into bamboo felt；
S6: by step S5 treated bamboo felt is put into nitrogen protection furnace progress medium temperature carbonization treatment；It later will be at medium temperature carbonization
Bamboo felt body after reason uniformly penetrates into the curing agent after dilution, and heat preservation solidification is formed in curing oven；Bamboo felt is sent into later and is carbonized
High temperature cabonization is carried out in reacting furnace, obtains bamboo carbon felt；
S7: bamboo carbon felt obtained by step S6 is subjected to CVD processing；
S8: by step S7, treated that bamboo carbon felt is put into high temperature furnace carries out high-temperature process, obtains the solidification carbon felt.
3. a kind of preparation method of environment-friendly solidified carbon felt as claimed in claim 2, which is characterized in that in the step S1, institute
Stating bamboo is diameter >=10cm bamboo；The degumming agent is NaHCO3、Na2CO3Or NaOH is one such；Described impregnate takes off
Glue is 3~5h of heat-insulation soaking at 90~110 DEG C.
4. a kind of preparation method of environment-friendly solidified carbon felt as claimed in claim 2, which is characterized in that in the step S2, institute
The mass fraction for stating concentrated hydrochloric acid is 20%-38%；It is described to impregnate to impregnate 20~40min at room temperature.
5. a kind of preparation method of environment-friendly solidified carbon felt as claimed in claim 2, which is characterized in that in the step S3, institute
The mass fraction for stating dilute hydrochloric acid is 10%~20%；The temperature of the heating and thermal insulation is < 80 DEG C；It is described pressurization pressure maintaining pressure be
1.4~1.6MPa；The time of the heat-insulation pressure keeping is 5~8h.
6. a kind of preparation method of environment-friendly solidified carbon felt as claimed in claim 2, which is characterized in that in the step S4, institute
Stating softening agent is one of sulfonated oil or silicone oil；The time that the softening is impregnated is 1~5h；The temperature of the drying is 200
~260 DEG C, the time is 4~6h.
7. a kind of preparation method of environment-friendly solidified carbon felt as claimed in claim 2, which is characterized in that in the step S5, often
Dust and impurities will be shrugged off after the secondary shredding；The needle set of the shredding is made of bamboo stick.
8. a kind of preparation method of environment-friendly solidified carbon felt as claimed in claim 2, which is characterized in that in the step S6, institute
The temperature for stating medium temperature carbonization treatment is 500 DEG C~800 DEG C, and the time is 10~20h；The curing agent includes colloid or resin；Institute
Stating diluent used by dilution is alcohol or methanol；The temperature of the solidifying and setting is 150~250 DEG C, and the time is 5~10h；
The temperature of the high temperature cabonization is 1100~1400 DEG C, and the time is 5~20h.
9. a kind of preparation method of environment-friendly solidified carbon felt as claimed in claim 2, which is characterized in that in the step S7, institute
The temperature for stating CVD processing is 950~1050 DEG C, and the time is 10~20h, and carbon-source gas is in natural gas, methane or propane gas
One kind.
10. a kind of preparation method of environment-friendly solidified carbon felt as claimed in claim 2, which is characterized in that in the step S8, institute
The temperature for stating high-temperature process is 2000~2500 DEG C, and the time is 5~10h.
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| CN112376267A (en) * | 2020-10-19 | 2021-02-19 | 安徽弘昌新材料有限公司 | Preparation method of cured carbon felt |
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