CN108411407A - A kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology - Google Patents
A kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology Download PDFInfo
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- CN108411407A CN108411407A CN201810234532.XA CN201810234532A CN108411407A CN 108411407 A CN108411407 A CN 108411407A CN 201810234532 A CN201810234532 A CN 201810234532A CN 108411407 A CN108411407 A CN 108411407A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
- D01F9/15—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues from coal pitch
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
- D01F9/155—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues from petroleum pitch
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H5/00—Non woven fabrics formed of mixtures of relatively short fibres and yarns or like filamentary material of substantial length
- D04H5/02—Non woven fabrics formed of mixtures of relatively short fibres and yarns or like filamentary material of substantial length strengthened or consolidated by mechanical methods, e.g. needling
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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
- D04H5/00—Non woven fabrics formed of mixtures of relatively short fibres and yarns or like filamentary material of substantial length
- D04H5/08—Non woven fabrics formed of mixtures of relatively short fibres and yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of fibres or yarns
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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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Inorganic Fibers (AREA)
Abstract
The present invention provides the preparation methods that a kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology includes long fine carbon fiber, the preparation method of the preparation method of the preparation method and carbon carbon insulation quilt of short fibre carbon fiber, long fibre carbon fiber and short fine carbon fiber is respectively by raw material mixing, spinning, pre-oxidation treatment, carbonization；The preparation method of carbon carbon insulation quilt is long fine carbon fiber and short fine carbon fiber mixing, forms web tire, needling shape networking tire unit, hot setting processing, high temperature cabonization processing.The present invention recycles 2 kinds of carbon fibers to prepare carbon carbon insulation quilt by preparing long fine, short fine carbon fiber, prepares that density is relatively low, and Density Distribution is uniform, and heat insulation property is good, lower-cost carbon carbon insulation quilt.
Description
Technical field
The invention belongs to carbon fibre material preparing technical field more particularly to a kind of long fine, short fine mixed type carbon carbon heat preservations
Felt processing technology.
Background technology
Carbon carbon composite is carbon fiber and its carbon-based composite material of fabric enhancing, has low-density, high intensity, height
Than mould, low ablating rate, high-heat resistance shock resistant, low thermal coefficient of expansion, zero hygral expansion, do not deflate, the intensity and modulus within 2000 DEG C
With temperature raising, increase, good anti-fatigue performance, beneficial friction and wear behavior and biocompatibility, especially carbon carbon are multiple
The special performance that condensation material intensity goes up not down with the raising of temperature, makes it as high-performance enginer hot-end component and use
There is the advantage that other materials hardly match in hypersonic aircraft thermal protection system.In recent years, with carbon fiber raw material
And its reduction of manufacturing cost, carbon carbon composite is not only in aerospace field, also in industrial circle, such as traffic, machine
Application in tool, sports and amusement, leisure goods, health care and civil construction etc. is more and more extensive.
Carbon fiber thermal insulation felt is a kind of adiabatic heat-insulation functional material applied under vacuum or inert atmosphere, is answered extensively
For gaseous phase deposition stove, monocrystal growing furnace, polycrystalline foundry furnace, polycrystalline reduction furnace, vacuum sintering furnace, hot pressing furnace, thermal balance stove, electricity
High-end insulation material, carbon fiber are used as in the nonoxidizing atmospheres high-temperature services such as magnetic induction stove, HIGH-PURITY SILICON hydrogenation furnace, vacuum smelting furnace
Insulation quilt suffers from the energy-saving and emission-reduction of product quality, purity and the equipment produced, safe operating environment of equipment etc.
Very important effect.The short fine carbon fiber of current Carbon fiber thermal insulation felt generally use is processed manufacture, manufacturing cost is excessively high,
The defects of yield is relatively low and technology is excessively complicated restricts the development of carbon fiber industry.
101591178 B of patent CN disclose manufacture and the surface treatment side of a kind of rigid carbon-fiber heat-insulation material
Ground carbon fiber and binder and dispersant solution are sufficiently mixed by method, through vacuum filtration or compression molding, by non-fusible
And carbonization treatment, obtained rigid carbon-fiber thermal insulation material, binder easily accumulate in the surface of moulding material, and gained is caused to produce
Product center lacks cohesive force, easy to crack；And density is big, Density Distribution is uneven, thermal and insulating performance is poor, and cost is higher.
Invention content
In order to solve problems in the prior art, the present invention provides a kind of long fine, short fine mixed type carbon carbon insulation quilt processing
Technique recycles 2 kinds of carbon fibers to prepare carbon carbon insulation quilt by preparing long fine, short fine carbon fiber, and it is relatively low to prepare density, close
Degree is evenly distributed, and heat insulation property is good, lower-cost carbon carbon insulation quilt.
In order to achieve the above object, the present invention provides following technical scheme：
A kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology includes the preparation method of long fine carbon fiber, short fibre carbon
The preparation method of the preparation method and carbon carbon insulation quilt of fiber, is as follows：
1. the preparation method of the fine carbon fiber of length includes the following steps：
(1) it is 1 according to mass ratio by coal tar pitch and asphalt:1 mixing, and it is heated to molten under nitrogen protection
State, heating temperature are 560-600 DEG C, then heating time 0.5-1h is stirred 1-1.5h at 100-180 DEG C, obtains
Mix asphalt raw material；
(2) raw material of following mass fraction is mixed：60-75 parts of mix asphalt raw material, 3,4,9,10- tetracarboxylic acid dianhydrides
1-3 parts, 1-2 parts of Alkylphenyl polysiloxane, 1-3 parts of pitch viscosity reductant, 5-9 parts of polyphenylene sulfide, polyamide 6-12
11-20 parts of part and methacrylonitrile heat 1h, obtain spinning mixture at 280-350 DEG C；
(3) spinning mixture is put into melt spinning machine machine spinneret barrel, be packed into carbon fiber device for spinning, with 5-8 DEG C/
The Elevated Temperature Conditions of min rise to 430-450 DEG C, then are down to 190-210 DEG C with the decrease speed of 1-3 DEG C/min, you can in spinneret
Mouth obtains precursor；
(4) under the protection of nitrogen, precursor is subjected to pre-oxidation treatment, the medium of pre-oxidation is hydrogen peroxide, in 360-400
DEG C heat treatment 20-35min；
(5) precursor after pre-oxidation treatment that step (4) obtains is subjected to heating carbonization, the temperature of heating is 1200-
1450 DEG C, the time of heating is 1-2h, obtains long fine carbon fiber；
Preferably, the pitch viscosity reductant in acrylic resin, polyacrylamide and ethylene bis stearamide one
Kind is a variety of.
Preferably, the weight average molecular weight of the polyphenylene sulfide is 40000-50000；The Weight-average molecular of polyamide
Amount is 2000-4000.
Preferably, a length of 300-700mm of fiber of the long fine carbon fiber.
2. the preparation method of short fibre carbon fiber includes the following steps：
(1) it is 1 according to mass ratio by coal tar pitch and asphalt:2 mixing, and it is heated to molten under nitrogen protection
State, heating temperature are 560-600 DEG C, then heating time 0.5-1h is stirred 1-1.5h at 100-180 DEG C, obtains
Mix asphalt raw material；
(2) raw material of following mass fraction is mixed：60-75 parts of mix asphalt raw material, 0.5-1 parts of 2,6- naphthalenedicarboxylic acids,
12-20 parts of 1-3 parts of pitch viscosity reductant, 5-9 parts of polyvinyl resin, 6-13 parts of acrylic resin and methacrylonitrile mixing,
At 280-350 DEG C, 1h is heated, spinning mixture is obtained；
(3) spinning mixture is put into melt spinning machine machine spinneret barrel, be packed into carbon fiber device for spinning, with 5-8 DEG C/
The Elevated Temperature Conditions of min rise to 430-450 DEG C, then are down to 190-210 DEG C with the decrease speed of 1-3 DEG C/min, you can in spinneret
Mouth obtains precursor；
(4) under the protection of nitrogen, precursor is subjected to pre-oxidation treatment, the medium of pre-oxidation is hydrogen peroxide, in 360-400
DEG C heat treatment 20-35min；
(5) precursor after pre-oxidation treatment that step (4) obtains is subjected to heating carbonization, the temperature of heating is 1200-
1450 DEG C, the time of heating is 1-2h, obtains short fine carbon fiber；
Preferably, the pitch viscosity reductant in acrylic resin, polyacrylamide and ethylene bis stearamide one
Kind is a variety of.
Preferably, the weight average molecular weight of the polyvinyl resin is 5000-6000；The weight average molecular weight of acrylic resin is
7000-9000。
Preferably, a length of 10-290mm of fiber of the short fine carbon fiber.
3. the preparation method of carbon carbon insulation quilt includes the following steps：
(1) it is 3 according to weight ratio by long fine carbon fiber and short fine carbon fiber:7-5:5 are mixed, and mixing carbon fiber is obtained
Dimension；
(2) it is 500-2000g/m by airlaid formation grammes per square metre by mixed carbon fibre2Web tire；
(3) 2-10 layers of web tire needle thorn are combined into a net tire unit using needle-punching method, the density of needle thorn is 2-
15 needles/cm2；
(4) curing process is carried out to net tire unit, net tire unit is placed in high-pressure molding mold, pressure 2- is forced into
6MPa keeps the temperature 1-2h under conditions of 100-120 DEG C, and 1-2h is kept the temperature under conditions of then heating to 150-170 DEG C, is heated up later
2-5h is kept the temperature under the conditions of to 200-230 DEG C, finally naturally cools to 70-90 DEG C；
(5) the net tire unit after step (4) curing process is subjected to high temperature cabonization processing, under nitrogen atmosphere, by step
(4) carbonization treatment 1.5-2h under the conditions of temperature is 700-900 DEG C of the net tire unit after curing process, then heats to 1500-
1700 DEG C of heat preservation 0.5-1h, last cooled to room temperature obtain long fine, short fine mixed type carbon carbon insulation quilt.
Preferably, the preparation method of web tire is as follows in the step (2)：Mixed carbon fibre 90 is weighed by mass fraction
Part, 0.5 part of methylcellulose, 0.5 part of polyacrylamide, 3000 parts of water are dispersed with stirring uniformly, pour into suction filtration mold, suction filtration is gone
Water removal, under the conditions of temperature is 80-120 DEG C, it is 500-2000g/m that drying, which obtains grammes per square metre,2Web tire.
Using above-mentioned technical proposal, what the present invention realized has the beneficial effect that：
(1) present invention prepares long fine carbon fiber and short fine carbon fiber respectively, is prepared without that will grow fine carbon fiber cutting
At short fine carbon fiber so that the tensile strength of long fibre carbon fiber and short fine carbon fiber is big.
(2) Density Distribution for the carbon carbon insulation quilt that the present invention is mixed with by long fine carbon fiber and short fine carbon fiber is uniform,
Density is small, and heat insulation property is good, at low cost.
(3) hardness of long fine, short fine mixed type carbon carbon insulation quilt prepared by the present invention is moderate, easily processed into type.
Specific implementation mode
It is further illustrated the present invention with reference to embodiment.
Embodiment 1
A kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology includes the preparation method of long fine carbon fiber, short fibre carbon
The preparation method of the preparation method and carbon carbon insulation quilt of fiber, is as follows：
1. the preparation method of the fine carbon fiber of length includes the following steps：
(1) it is 1 according to mass ratio by coal tar pitch and asphalt:1 mixing, and it is heated to molten under nitrogen protection
State, heating temperature are 560 DEG C, and then heating time 1h is stirred 1h at 100 DEG C, obtain mix asphalt raw material；
(2) raw material of following mass fraction is mixed：75 parts of mix asphalt raw material, 3,4,9,10- tetracarboxylic acid dianhydrides 1
Part, 1 part of Alkylphenyl polysiloxane, 1 part of pitch viscosity reductant, 5 parts of polyphenylene sulfide, 6 parts of polyamide and metering system
11 parts of nitrile heats 1h, obtains spinning mixture at 280 DEG C；
(3) spinning mixture is put into melt spinning machine machine spinneret barrel, be packed into carbon fiber device for spinning, with 5 DEG C/
The Elevated Temperature Conditions of min rise to 430 DEG C, then are down to 190 DEG C with the decrease speed of 1 DEG C/min, you can obtain precursor in spinning nozzle；
(4) under the protection of nitrogen, precursor is subjected to pre-oxidation treatment, the medium of pre-oxidation is hydrogen peroxide, in 360 DEG C of heat
Handle 20min；
(5) precursor after pre-oxidation treatment that step (4) obtains being subjected to heating carbonization, the temperature of heating is 1200 DEG C,
The time of heating is 2h, obtains long fine carbon fiber；
The pitch viscosity reductant is acrylic resin.
The weight average molecular weight of the polyphenylene sulfide is 42000；The weight average molecular weight of polyamide is 2000.
The a length of 300mm of fiber of the long fine carbon fiber.
2. the preparation method of short fibre carbon fiber includes the following steps：
(1) it is 1 according to mass ratio by coal tar pitch and asphalt:2 mixing, and it is heated to molten under nitrogen protection
State, heating temperature are 560 DEG C, and then heating time 1h is stirred 1h at 100 DEG C, obtain mix asphalt raw material；
(2) raw material of following mass fraction is mixed：75 parts of mix asphalt raw material, 1 part of 2,6- naphthalenedicarboxylic acids, pitch visbreaking
12 parts of 1 part of agent, 5 parts of polyvinyl resin, 6 parts of acrylic resin and methacrylonitrile mixing are heated 1h, are spun at 280 DEG C
Silk mixture；
(3) spinning mixture is put into melt spinning machine machine spinneret barrel, be packed into carbon fiber device for spinning, with 5 DEG C/
The Elevated Temperature Conditions of min rise to 430 DEG C, then are down to 190 DEG C with the decrease speed of 1 DEG C/min, you can obtain precursor in spinning nozzle；
(4) under the protection of nitrogen, precursor is subjected to pre-oxidation treatment, the medium of pre-oxidation is hydrogen peroxide, in 360 DEG C of heat
Handle 20min；
(5) precursor after pre-oxidation treatment that step (4) obtains being subjected to heating carbonization, the temperature of heating is 1200 DEG C,
The time of heating is 1h, obtains short fine carbon fiber；
The pitch viscosity reductant is acrylic resin.
The weight average molecular weight of the polyvinyl resin is 5000；The weight average molecular weight of acrylic resin is 7000.
Preferably, a length of 10mm of fiber of the short fine carbon fiber.
3. the preparation method of carbon carbon insulation quilt includes the following steps：
(1) it is 3 according to weight ratio by long fine carbon fiber and short fine carbon fiber:7 are mixed, and mixed carbon fibre is obtained；
(2) it is 500g/m by airlaid formation grammes per square metre by mixed carbon fibre2Web tire；
(3) 10 layers of web tire needle thorn is combined into a net tire unit using needle-punching method, the density of needle thorn be 15 needles/
cm2；
(4) curing process is carried out to net tire unit, net tire unit is placed in high-pressure molding mold, pressure is forced into
6MPa keeps the temperature 1h under conditions of 100 DEG C, 1h is kept the temperature under conditions of then heating to 150 DEG C, is warming up to 200 DEG C of conditions later
Lower heat preservation 2h, finally naturally cools to 70 DEG C；
(5) the net tire unit after step (4) curing process is subjected to high temperature cabonization processing, under nitrogen atmosphere, by step
(4) carbonization treatment 1.5h under the conditions of temperature is 700 DEG C of the net tire unit after curing process, then heats to 1500 DEG C of heat preservations
0.5h, last cooled to room temperature obtain long fine, short fine mixed type carbon carbon insulation quilt.
The preparation method of web tire is as follows in the step (2)：90 parts of mixed carbon fibre, methyl are weighed by mass fraction
0.5 part of cellulose, 0.5 part of polyacrylamide, 3000 parts of water are dispersed with stirring uniformly, pour into suction filtration mold, and suction filtration goes to remove water,
Under the conditions of temperature is 80 DEG C, it is 500g/m that drying, which obtains grammes per square metre,2Web tire.
Embodiment 2
A kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology includes the preparation method of long fine carbon fiber, short fibre carbon
The preparation method of the preparation method and carbon carbon insulation quilt of fiber, is as follows：
1. the preparation method of the fine carbon fiber of length includes the following steps：
(1) it is 1 according to mass ratio by coal tar pitch and asphalt:1 mixing, and it is heated to molten under nitrogen protection
State, heating temperature are 600 DEG C, and then heating time 0.5h is stirred 1.5h at 180 DEG C, obtain mix asphalt raw material；
(2) raw material of following mass fraction is mixed：60 parts of mix asphalt raw material, 3,4,9,10- tetracarboxylic acid dianhydrides 3
Part, 2 parts of Alkylphenyl polysiloxane, 3 parts of pitch viscosity reductant, 9 parts of polyphenylene sulfide, 10 parts of polyamide and metering system
13 parts of nitrile heats 1h, obtains spinning mixture at 350 DEG C；
(3) spinning mixture is put into melt spinning machine machine spinneret barrel, be packed into carbon fiber device for spinning, with 8 DEG C/
The Elevated Temperature Conditions of min rise to 450 DEG C, then are down to 210 DEG C with the decrease speed of 3 DEG C/min, you can obtain precursor in spinning nozzle；
(4) under the protection of nitrogen, precursor is subjected to pre-oxidation treatment, the medium of pre-oxidation is hydrogen peroxide, in 400 DEG C of heat
Handle 35min；
(5) precursor after pre-oxidation treatment that step (4) obtains being subjected to heating carbonization, the temperature of heating is 1450 DEG C,
The time of heating is 1h, obtains long fine carbon fiber；
The pitch viscosity reductant is the mixture of acrylic resin and polyacrylamide.
The weight average molecular weight of the polyphenylene sulfide is 50000；The weight average molecular weight of polyamide is 4000.
Preferably, a length of 700mm of fiber of the long fine carbon fiber.
2. the preparation method of short fibre carbon fiber includes the following steps：
(1) it is 1 according to mass ratio by coal tar pitch and asphalt:2 mixing, and it is heated to molten under nitrogen protection
State, heating temperature are 600 DEG C, and then heating time 0.5h is stirred 1.5h at 180 DEG C, obtain mix asphalt raw material；
(2) raw material of following mass fraction is mixed：60 parts of mix asphalt raw material, 0.5 part of 2,6- naphthalenedicarboxylic acids, pitch subtract
14.5 parts of 3 parts of stick, 9 parts of polyvinyl resin, 13 parts of acrylic resin and methacrylonitrile mixing heat 1h at 350 DEG C,
Obtain spinning mixture；
(3) spinning mixture is put into melt spinning machine machine spinneret barrel, be packed into carbon fiber device for spinning, with 8 DEG C/
The Elevated Temperature Conditions of min rise to 450 DEG C, then are down to 210 DEG C with the decrease speed of 3 DEG C/min, you can obtain precursor in spinning nozzle；
(4) under the protection of nitrogen, precursor is subjected to pre-oxidation treatment, the medium of pre-oxidation is hydrogen peroxide, in 400 DEG C of heat
Handle 35min；
(5) precursor after pre-oxidation treatment that step (4) obtains being subjected to heating carbonization, the temperature of heating is 1450 DEG C,
The time of heating is 2h, obtains short fine carbon fiber；
The pitch viscosity reductant is the mixture of acrylic resin and polyacrylamide.
The weight average molecular weight of the polyvinyl resin is 6000；The weight average molecular weight of acrylic resin is 9000.
The a length of 290mm of fiber of the short fine carbon fiber.
3. the preparation method of carbon carbon insulation quilt includes the following steps：
(1) it is 5 according to weight ratio by long fine carbon fiber and short fine carbon fiber:5 are mixed, and mixed carbon fibre is obtained；
(2) it is 2000g/m by airlaid formation grammes per square metre by mixed carbon fibre2Web tire；
(3) 2 layers of web tire needle thorn is combined into a net tire unit using needle-punching method, the density of needle thorn be 2 needles/
cm2；
(4) curing process is carried out to net tire unit, net tire unit is placed in high-pressure molding mold, pressure is forced into
2MPa keeps the temperature 2h under conditions of 120 DEG C, 2h is kept the temperature under conditions of then heating to 170 DEG C, is warming up to 230 DEG C of conditions later
Lower heat preservation 5h, finally naturally cools to 90 DEG C；
(5) the net tire unit after step (4) curing process is subjected to high temperature cabonization processing, under nitrogen atmosphere, by step
(4) carbonization treatment 2h under the conditions of temperature is 900 DEG C of the net tire unit after curing process then heats to 1700 DEG C of heat preservation 1h,
Last cooled to room temperature obtains long fine, short fine mixed type carbon carbon insulation quilt.
The preparation method of web tire is as follows in the step (2)：90 parts of mixed carbon fibre, methyl are weighed by mass fraction
0.5 part of cellulose, 0.5 part of polyacrylamide, 3000 parts of water are dispersed with stirring uniformly, pour into suction filtration mold, and suction filtration goes to remove water,
Under the conditions of temperature is 120 DEG C, it is 2000g/m that drying, which obtains grammes per square metre,2Web tire.
Embodiment 3
A kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology includes the preparation method of long fine carbon fiber, short fibre carbon
The preparation method of the preparation method and carbon carbon insulation quilt of fiber, is as follows：
1. the preparation method of the fine carbon fiber of length includes the following steps：
(1) it is 1 according to mass ratio by coal tar pitch and asphalt:1 mixing, and it is heated to molten under nitrogen protection
State, heating temperature are 560 DEG C, and then heating time 1h is stirred 1h at 180 DEG C, obtain mix asphalt raw material；
(2) raw material of following mass fraction is mixed：60 parts of mix asphalt raw material, 3,4,9,10- tetracarboxylic acid dianhydrides 1
Part, 1 part of Alkylphenyl polysiloxane, 1 part of pitch viscosity reductant, 5 parts of polyphenylene sulfide, 12 parts of polyamide and metering system
20 parts of nitrile heats 1h, obtains spinning mixture at 350 DEG C；
(3) spinning mixture is put into melt spinning machine machine spinneret barrel, be packed into carbon fiber device for spinning, with 8 DEG C/
The Elevated Temperature Conditions of min rise to 450 DEG C, then are down to 210 DEG C with the decrease speed of 3 DEG C/min, you can obtain precursor in spinning nozzle；
(4) under the protection of nitrogen, precursor is subjected to pre-oxidation treatment, the medium of pre-oxidation is hydrogen peroxide, in 360 DEG C of heat
Handle 35min；
(5) precursor after pre-oxidation treatment that step (4) obtains being subjected to heating carbonization, the temperature of heating is 1200 DEG C,
The time of heating is 2h, obtains long fine carbon fiber；
The pitch viscosity reductant is ethylene bis stearamide.
The weight average molecular weight of the polyphenylene sulfide is 40000；The weight average molecular weight of polyamide is 4000.
The a length of 400mm of fiber of the long fine carbon fiber.
2. the preparation method of short fibre carbon fiber includes the following steps：
(1) it is 1 according to mass ratio by coal tar pitch and asphalt:2 mixing, and it is heated to molten under nitrogen protection
State, heating temperature are 560 DEG C, and then heating time 1h is stirred 1h at 180 DEG C, obtain mix asphalt raw material；
(2) raw material of following mass fraction is mixed：65 parts of mix asphalt raw material, 1 part of 2,6- naphthalenedicarboxylic acids, pitch visbreaking
20 parts of 3 parts of agent, 5 parts of polyvinyl resin, 6 parts of acrylic resin and methacrylonitrile mixing are heated 1h, are spun at 350 DEG C
Silk mixture；
(3) spinning mixture is put into melt spinning machine machine spinneret barrel, be packed into carbon fiber device for spinning, with 5 DEG C/
The Elevated Temperature Conditions of min rise to 430 DEG C, then are down to 190 DEG C with the decrease speed of 1 DEG C/min, you can obtain precursor in spinning nozzle；
(4) under the protection of nitrogen, precursor is subjected to pre-oxidation treatment, the medium of pre-oxidation is hydrogen peroxide, in 400 DEG C of heat
Handle 20min；
(5) precursor after pre-oxidation treatment that step (4) obtains being subjected to heating carbonization, the temperature of heating is 1200 DEG C,
The time of heating is 2h, obtains short fine carbon fiber；
The pitch viscosity reductant is ethylene bis stearamide.
The weight average molecular weight of the polyvinyl resin is 5000；The weight average molecular weight of acrylic resin is 7000.
The a length of 100mm of fiber of the short fine carbon fiber.
3. the preparation method of carbon carbon insulation quilt includes the following steps：
(1) it is 4 according to weight ratio by long fine carbon fiber and short fine carbon fiber:6 are mixed, and mixed carbon fibre is obtained；
(2) it is 1000g/m by airlaid formation grammes per square metre by mixed carbon fibre2Web tire；
(3) 5 layers of web tire needle thorn is combined into a net tire unit using needle-punching method, the density of needle thorn be 7 needles/
cm2；
(4) curing process is carried out to net tire unit, net tire unit is placed in high-pressure molding mold, pressure is forced into
4MPa keeps the temperature 2h under conditions of 100 DEG C, 2h is kept the temperature under conditions of then heating to 150 DEG C, is warming up to 230 DEG C of conditions later
Lower heat preservation 2h, finally naturally cools to 70 DEG C；
(5) the net tire unit after step (4) curing process is subjected to high temperature cabonization processing, under nitrogen atmosphere, by step
(4) carbonization treatment 2h under the conditions of temperature is 700 DEG C of the net tire unit after curing process then heats to 1500 DEG C of heat preservation 1h,
Last cooled to room temperature obtains long fine, short fine mixed type carbon carbon insulation quilt.
The preparation method of web tire is as follows in the step (2)：90 parts of mixed carbon fibre, methyl are weighed by mass fraction
0.5 part of cellulose, 0.5 part of polyacrylamide, 3000 parts of water are dispersed with stirring uniformly, pour into suction filtration mold, and suction filtration goes to remove water,
Under the conditions of temperature is 120 DEG C, it is 1000g/m that drying, which obtains grammes per square metre,2Web tire.
Although above-mentioned be described the specific implementation mode of the present invention in conjunction with the embodiments, not the present invention is protected
The limitation of range, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art
The various modifications or changes that can be made need not be made the creative labor still within protection scope of the present invention.
Claims (7)
1. a kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology, it is characterised in that：Include the preparation side of long fine carbon fiber
Method, the preparation method of the preparation method and carbon carbon insulation quilt of short fibre carbon fiber, is as follows：
The preparation method of long fibre carbon fiber includes the following steps：
(1) it is 1 according to mass ratio by coal tar pitch and asphalt:1 mixing, and it is heated to molten condition under nitrogen protection,
Heating temperature is 560-600 DEG C, then heating time 0.5-1h is stirred 1-1.5h at 100-180 DEG C, is mixed
Asphalt stock；
(2) raw material of following mass fraction is mixed：60-75 parts of mix asphalt raw material, 3,4,9,10- tetracarboxylic acid dianhydrides 1-3
Part, 1-2 parts of Alkylphenyl polysiloxane, 1-3 parts of pitch viscosity reductant, 5-9 parts of polyphenylene sulfide, 6-12 parts of polyamide and
11-20 parts of methacrylonitrile heats 1h, obtains spinning mixture at 280-350 DEG C；
(3) spinning mixture is put into melt spinning machine machine spinneret barrel, carbon fiber device for spinning is packed into, with 5-8 DEG C/min
Elevated Temperature Conditions rise to 430-450 DEG C, then be down to 190-210 DEG C with the decrease speed of 1-3 DEG C/min, you can obtain in spinning nozzle
To precursor；
(4) under the protection of nitrogen, precursor is subjected to pre-oxidation treatment, the medium of pre-oxidation is hydrogen peroxide, in 360-400 DEG C of heat
Handle 20-35min；
(5) precursor after pre-oxidation treatment that step (4) obtains being subjected to heating carbonization, the temperature of heating is 1200-1450 DEG C,
The time of heating is 1-2h, obtains long fine carbon fiber；
The preparation method of short fibre carbon fiber includes the following steps：
(1) it is 1 according to mass ratio by coal tar pitch and asphalt:2 mixing, and it is heated to molten condition under nitrogen protection,
Heating temperature is 560-600 DEG C, then heating time 0.5-1h is stirred 1-1.5h at 100-180 DEG C, is mixed
Asphalt stock；
(2) raw material of following mass fraction is mixed：60-75 parts of mix asphalt raw material, 0.5-1 parts of 2,6- naphthalenedicarboxylic acids, pitch
12-20 parts of 1-3 parts of viscosity reductant, 5-9 parts of polyvinyl resin, 6-13 parts of acrylic resin and methacrylonitrile mixing, in 280-350
At DEG C, 1h is heated, spinning mixture is obtained；
(3) spinning mixture is put into melt spinning machine machine spinneret barrel, carbon fiber device for spinning is packed into, with 5-8 DEG C/min
Elevated Temperature Conditions rise to 430-450 DEG C, then be down to 190-210 DEG C with the decrease speed of 1-3 DEG C/min, you can obtain in spinning nozzle
To precursor；
(4) under the protection of nitrogen, precursor is subjected to pre-oxidation treatment, the medium of pre-oxidation is hydrogen peroxide, in 360-400 DEG C of heat
Handle 20-35min；
(5) precursor after pre-oxidation treatment that step (4) obtains being subjected to heating carbonization, the temperature of heating is 1200-1450 DEG C,
The time of heating is 1-2h, obtains short fine carbon fiber；
The preparation method of carbon carbon insulation quilt includes the following steps：
(1) it is 3 according to weight ratio by long fine carbon fiber and short fine carbon fiber:7-5:5 are mixed, and mixed carbon fibre is obtained；
(2) it is 500-2000g/m by airlaid formation grammes per square metre by mixed carbon fibre2Web tire；
(3) 2-10 layers of web tire needle thorn is combined into a net tire unit using needle-punching method, the density of needle thorn be 2-15 needles/
cm2；
(4) curing process is carried out to net tire unit, net tire unit is placed in high-pressure molding mold, pressure 2- is forced into
6MPa keeps the temperature 1-2h under conditions of 100-120 DEG C, and 1-2h is kept the temperature under conditions of then heating to 150-170 DEG C, is heated up later
2-5h is kept the temperature under the conditions of to 200-230 DEG C, finally naturally cools to 70-90 DEG C；
(5) the net tire unit after step (4) curing process is subjected to high temperature cabonization processing, it is under nitrogen atmosphere, step (4) are solid
Change treated net tire unit carbonization treatment 1.5-2h under the conditions of temperature is 700-900 DEG C, then heats to 1500-1700 DEG C
0.5-1h is kept the temperature, last cooled to room temperature obtains long fine, short fine mixed type carbon carbon insulation quilt.
2. a kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology according to claim 1, it is characterised in that：Institute
It is one or more in acrylic resin, polyacrylamide and ethylene bis stearamide to state pitch viscosity reductant.
3. a kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology according to claim 1, it is characterised in that：Institute
The weight average molecular weight for stating polyphenylene sulfide is 40000-50000；The weight average molecular weight of polyamide is 2000-4000.
4. a kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology according to claim 1, it is characterised in that：Institute
The weight average molecular weight for stating polyvinyl resin is 5000-6000；The weight average molecular weight of acrylic resin is 7000-9000.
5. a kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology according to claim 1, it is characterised in that：Institute
State a length of 300-700mm of fiber of long fine carbon fiber.
6. a kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology according to claim 1, it is characterised in that：Institute
State a length of 10-290mm of fiber of short fine carbon fiber.
7. a kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology according to claim 1, it is characterised in that：Institute
The preparation method of web tire is as follows in the step of stating the preparation method of carbon carbon insulation quilt (2)：Mixing carbon is weighed by mass fraction
90 parts of fiber, 0.5 part of methylcellulose, 0.5 part of polyacrylamide, 3000 parts of water are dispersed with stirring uniformly, pour into suction filtration mold,
Suction filtration goes to remove water, and under the conditions of temperature is 80-120 DEG C, it is 500-2000g/m that drying, which obtains grammes per square metre,2Web tire.
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| CN109688643A (en) * | 2019-01-09 | 2019-04-26 | 嘉兴启晟碳材料有限公司 | A kind of carbon carbon heater and its manufacturing process |
| CN110725068A (en) * | 2019-11-27 | 2020-01-24 | 南京得贝利新型材料有限责任公司 | Carbon fiber felt production process based on carbon fiber waste filaments |
| CN111636143A (en) * | 2020-05-28 | 2020-09-08 | 山东奥达复合材料有限公司 | Three-dimensional felt of carbon fiber |
| CN113026349A (en) * | 2021-03-12 | 2021-06-25 | 上海瑟赫新材料科技有限公司 | Heat-preserving and heat-insulating carbon felt and preparation method thereof |
| CN114645376A (en) * | 2022-05-13 | 2022-06-21 | 浙江星辉新材料科技有限公司 | Preparation method of low-density carbon fiber hard heat-preservation felt |
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| CN114645376A (en) * | 2022-05-13 | 2022-06-21 | 浙江星辉新材料科技有限公司 | Preparation method of low-density carbon fiber hard heat-preservation felt |
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Application publication date: 20180817 |