CN105479829B - A kind of hard heat-insulated felt of low density carbon fiber and preparation method thereof - Google Patents

A kind of hard heat-insulated felt of low density carbon fiber and preparation method thereof Download PDF

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Publication number
CN105479829B
CN105479829B CN201610020474.1A CN201610020474A CN105479829B CN 105479829 B CN105479829 B CN 105479829B CN 201610020474 A CN201610020474 A CN 201610020474A CN 105479829 B CN105479829 B CN 105479829B
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net tire
carbon fiber
net
layer
low density
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CN105479829A (en
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郭建军
郭建明
杨艳文
刘二良
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Qingdao Gao Tai New Material Co Ltd
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Qingdao Gao Tai New Material Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/028—Net structure, e.g. spaced apart filaments bonded at the crossing points
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/06—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer characterised by a fibrous or filamentary layer mechanically connected, e.g. by needling to another layer, e.g. of fibres, of paper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
    • B32B9/007—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4209—Inorganic fibres
    • D04H1/4242—Carbon fibres
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2250/00—Layers arrangement
    • B32B2250/20—All layers being fibrous or filamentary
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B32B2262/106—Carbon fibres, e.g. graphite fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2305/00—Condition, form or state of the layers or laminate
    • B32B2305/10—Fibres of continuous length
    • B32B2305/20—Fibres of continuous length in the form of a non-woven mat
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2305/00—Condition, form or state of the layers or laminate
    • B32B2305/38—Meshes, lattices or nets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/302—Conductive
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/304—Insulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
    • B32B2309/02—Temperature
    • B32B2309/022—Temperature vs pressure profiles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
    • B32B2309/02—Temperature
    • B32B2309/025—Temperature vs time profiles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
    • B32B2309/12—Pressure
    • B32B2309/125—Pressure vs time profiles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2313/00—Elements other than metals
    • B32B2313/04—Carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2571/00—Protective equipment

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Inorganic Chemistry (AREA)
  • Nonwoven Fabrics (AREA)
  • Inorganic Fibers (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The present invention relates to a kind of preparation method of the hard heat-insulated felt of low density carbon fiber：Carbon fiber is chopped into 3 30mm, lousiness is combed into carding machine and net tire is made, 2 40 layers of net tire acupuncture are combined into a net tire unit using needle-punching method, the density of acupuncture is 2 50 pins/cm2；Single or double glue spraying is carried out to net tire unit obtained above using fog spraying method, the net tire unit after glue spraying and net tire unit or protecting film are laminated；Material after stacking obtains carbon fiber hard insulation quilt primary product through hot pressing, carbonization and purifying successively, then machined into high temperature furnace required product.The hard heat-insulated felt of low density carbon fiber being prepared by the above method, including some net tire elementary layers, it is bonded together between net tire elementary layer；The net tire elementary layer includes some net plies, is linked together between net plies by acupuncture.The preparation technology of the present invention is simple, and the insulation quilt density of preparation is low, and good heat insulating, cost is low, and use environment is wide.

Description

A kind of hard heat-insulated felt of low density carbon fiber and preparation method thereof
Technical field
The present invention relates to high-temperature vacuum insulating equipment insulation material, and in particular to a kind of hard heat-insulated felt of low density carbon fiber And preparation method thereof.
Background technology
As need to possess one of many high temperature furnace industries, photovoltaic polycrystalline silicon ingot casting, because equipment depreciation rate is high, by external city Field is low to be influenceed, and product profit is low, domestic every cost increase.It is one of photovoltaic industry life condition to reduce cost, as disappearing The heat-insulating heat-preserving material of one of part is consumed, consumes every year huge, the quality of its thermal and insulating performance directly affects the performance of enterprise.
Existing market high temperature insulating material uses side mutually compound containing miscellaneous soft felt, or using mixing casting Method.As CN101948327A, CN103568385A, its product produced, longitudinal fiber content are too high, heat insulation effect is not too much It is preferable.And existing carbon fiber hard insulation quilt uses carbon fiber mixing wet method vacuum filtration shaping in the slurry, as in State's patent application 201310489217.9, has that density is big, structure consolidation feature using insulation quilt made from wet moulding, and this Kind feature determines that its thermal and insulating performance is poor；And under same volume, the material that density height need to use is also more, therefore is produced into This is of a relatively high.
The content of the invention
In view of the above-mentioned problems, the present invention is intended to provide a kind of cost is lower, the more preferable low density carbon of heat insulating effect is fine Tie up hard heat-insulated felt and preparation method thereof.
A kind of preparation method of the hard heat-insulated felt of low density carbon fiber, step are as follows：
(1) using the carbon fiber of carbon content >=92% as raw material, carbon fiber is chopped into 3-30mm, hair is combed into carding machine Simultaneously net tire is made in silk, and net tire grammes per square metre is 20-400g/m2, thickness 0.2-200mm, density 0.08-0.2g/cm3, carbon fiber row Cloth direction and plane where net tire are basically identical；
(2) 2-40 layer net tire acupunctures are combined into a net tire unit using needle-punching method, the density of acupuncture for 2-50 pins/ cm2；
(3) single or double glue spraying is carried out to net tire unit obtained above using fog spraying method, glue spraying amount is 0.8-1.2kg/m2；
(4) the net tire unit after glue spraying and net tire unit or protecting film are laminated；
(5) after hot press being preheating into 110-120 DEG C, the material being laminated is placed in hot press at once, is forced into Pressure 3-5MPa, continue to raise hot press temperature to 195 DEG C, and keep after continuing 1-10 hours at a temperature of this, allow hot press from Less than 100 DEG C are so cooled to, product is taken out and prepares carbonization；
(6) upper step product is placed into carbonizing apparatus, sets heating curve, used time 3h is warming up to 300 DEG C, now led to Entering argon gas protection, used time 20h is warming up to 700 DEG C, then used time 3.5h is warming up to constant temperature 3-10 hours at 1050 DEG C, 1050 DEG C, from It is dynamic to be cooled to less than 60 DEG C, product is taken out and prepares high temperature purification；
(7) product after carbonization is placed in high temperature purification equipment, be evacuated to below 10 pas, set heating curve, used When 5h be warming up to 1050 DEG C, used time 6h is warming up to 1600 DEG C, and used time 6h is warming up to constant temperature 3-10 hours at 2200 DEG C, 2200 DEG C, Automatically less than 60 DEG C are cooled to, are drawn off obtaining carbon fiber hard insulation quilt primary product；
(8) above-mentioned primary product are machined into high temperature furnace required product.
Carbon fiber material in the step (1), it is that viscose, pitch, the fine, phenolic aldehyde of polypropylene etc. form for raw material carbonization Carbon fiber, its phosphorus content are 3-30mm after its length is chopped more than 92%, and longitudinal silk can be avoided by combing networking tire with carding machine Beam influences its effect of heat insulation, can also make product density as uniform as possible.
For above-mentioned net tire through step (2) acupuncture networking tire unit, needling direction is longitudinal direction, and net tire unit tiling direction is horizontal stroke To that is, needling direction is vertical with plane where net tire unit.Needling process quantity is unit area pricker number, is controlled in 2-50 Pin/cm2, make net tire fluffy.It must can cause to receive in product carbonization, pyroprocess when density is too low by specified pin number acupuncture Contracting relative density can increase, and when density is too high, its heat insulation effect can reduce.The present invention adopts in the preparation of net tire unit first With the method for low-density acupuncture, the quantity of longitudinal fiber can be greatly reduced, therefore heat-insulating property can be obviously improved.To the insulation quilt For, the heat insulation effect without acupuncture is best, but no acupuncture is difficult density to be done low, is possible to using acupuncture close Degree do it is low, therefore present invention employs reduce needling density mode.
Glue is low viscosity adhesive described in step (3), from one kind in phenolic resin, furane resins or bismaleimide resin Or it is a variety of, to spray.
The two-sided fog spraying of CNC high-pressure unit is carried out using numerical control glue sprayer in step (3), glue sprayer is provided with standby Shower nozzle, the specific feeding rate of shower nozzle and glue spraying amount are set according to product specification ratio.Conventional impregnate is replaced with the method for spraying Method, avoid adhesive be full of in carbon fiber gap so that finished product density is more suitable for heat insulation function, and heat-insulating property is more preferably. In the prior art to being combined into felt in addition to using dip bonding mode between carbon fibre web tire unit, also worn using high density Saturating needle-punching method, such as the A of CN 103568385.The present invention does not use acupuncture in this step, but uses glue spraying stacking multiple Close, avoid penetrate acupuncture cause longitudinal fiber heat conduction and heat radiation and make heat along needling direction export the defects of.
Protecting film includes 12k, 6k carbon cloth or 0.5-2mm graphite papers in step (4), and net tire unit is answered with these materials It can use, have the effect that under very environment after conjunction：One, buffer action, avoid gas or generation needed for body of heater production Gas enters in insulation material, causes mutually to pollute；Secondly, increase intensity, improve the anti-gas shock performance of product, improve insulation Plate service life；Thirdly, be easy to clean.
The mode of stacking includes net tire unit and the stacking of net tire unit in step (4), and the number of plies is 2-40 layers；Net tire unit with The number of plies of protecting film stacking of the same race or not of the same race, net tire unit and protecting film is at least 1 layer.
Machining in step (8) includes butt, circle, perforate, washes the mode such as thin.
The hard heat-insulated felt of low density carbon fiber being prepared by the above method, including some net tire elementary layers, net tire list It is bonded together between first layer；The net tire elementary layer includes some net plies, is linked together between net plies by acupuncture.
The net plies is combed by 3-30mm carbon fibers and formed, and carbon fiber direction and plane where net plies are basically identical. " basically identical " is due to that carbon fiber is very more, and it is flexible big, and because net plies has certain thickness, is combed Shi Buke can guarantee that each carbon fiber is all completely the same with plane where net plies, and certain some carbon fiber may be with the plane With certain angle；Furthermore during acupuncture, some carbon fibers inevitably become vertical with the trend of pin To, but generally most carbon fibers and plane where net plies are consistent, are avoided as far as possible in the presence of vertical with the plane Carbon fiber.In addition, become longitudinal carbon fiber with the trend of pin plays certain supporting role in net tire structure, maintain Its fluff structure, so as to strengthen heat insulation effect.
The net tire elementary layer can also be bonded together with protection film layer, and protecting film layer number is at least 1 layer.
The net tire elementary layer to one layer is intervally arranged with protecting the adhered arrangement mode of film layer to be one layer, also may be used Be one layer to multilayer be intervally arranged or multilayer to one layer be intervally arranged or above-mentioned three kinds of intervals row The random combine of mode for cloth.
The present invention is engaged in high temperature insulating material making for many years in our company, according to the pass of the thermal conductivity of carbon fiber and density Difference is held in connection property, and the heat conduction that carbon fiber is in diametric(al) and fiber is axial.Produced by test of many times above-mentioned low close Carbon fiber hard insulation quilt is spent, is had the advantage that：(1) material density is less than 0.07g/cm3, insulation quilt density is less than 0.16g/ cm3, less than the density of the general insulation quilt of in the market, therefore heat-insulating property is more preferable, and plant capacity loss declines；(2) contrast existing Product list is from density, and with the product of same volume, material therefor weight is small, therefore cost reduces；(3) in insulation quilt Longitudinal fiber content is few, well below the content in existing product, due to carbon fiber in diametric(al) and fiber axial direction Difference is held in heat conduction, therefore the existing product high compared to longitudinal fiber content, heat-insulating property greatly improve；(4) more net tires are used Unit is bonded into felt, and can be layered stop and penetrate prevents heat conduction；(5) use environment is wide, suitable for various vacuum atmosphere sintering furnaces, Glowing furnace and crystal growing furnace (such as monocrystal growing furnace), polycrystalline ingot furnace, carborundum, other high temperature of gallium nitride correlation are set It is standby；(6) the carbonization amount purity of product is high, therefore more resistance to ablation, anti-airflow scouring；(7) it is of the invention compared to wet moulding Preparation technology is simpler, and structure design is more reasonable；(8) due to eliminating the steps such as drying, the production cycle of the invention is more It is short, it can save for about 1/3rd time；(9) insulation quilt prepared by the present invention, heat insulating effect are incubated better than existing market Material, so that for 900 DEG C of heat-insulated target, insulation quilt of the present invention can improve 10-45 than the heat-insulating capability of in the market insulation quilt ℃。
Brief description of the drawings
The vertical section structural representation of insulation quilt made from Fig. 1 embodiments 1；
The vertical section structural representation of insulation quilt made from Fig. 2 embodiments 2；
The vertical section structural representation of insulation quilt made from Fig. 3 embodiments 3；
In figure, 1- graphite linings；2- glue spraying layers；3- net tire units；4- longitudinal directions carbon fiber；5- carbon fibre cloth layers.
Embodiment
The present invention is described in further details with reference to specific embodiment and accompanying drawing.
Embodiment 1
A kind of preparation method of the hard heat-insulated felt of low density carbon fiber, step are as follows：
(1) using the fine base carbon fibre of the polypropylene of carbon content >=92% as raw material, carbon fiber is chopped into 3-30mm, with combing Machine is combed into lousiness and net tire is made, and net tire grammes per square metre is 50g/m2, thickness 4mm, density 0.06g/cm3, carbon fiber arrangement side To with net tire where plane it is basically identical；
(2) 8 layers of net tire acupuncture are combined into a net tire unit using needle-punching method, the density of acupuncture for 3-30 pins/ cm2；Needling direction is longitudinal direction, and net tire unit tiling direction is laterally, i.e., needling direction is vertical with plane where net tire unit.
(3) single or double spraying phenolic resin adhesion is carried out to net tire unit obtained above using fog spraying method Agent, glue spraying amount are 1.2kg/m2；
(4) the net tire unit after 15 two-sided glue sprayings is laminated；
(5) after hot press being preheating into 115 DEG C, the material being laminated is placed in hot press at once, is forced into pressure 4MPa, continue to raise hot press temperature to 195 DEG C, and keep after continuing 5 hours at a temperature of this, allow hot press Temperature fall to arrive Less than 100 DEG C, take out product and prepare carbonization；
(6) upper step product is placed into carbonizing apparatus, sets heating curve, used time 3h is warming up to 300 DEG C, now led to Enter argon gas protection, used time 20h is warming up to 700 DEG C, then used time 3.5h is warming up to constant temperature 6 hours at 1050 DEG C, 1050 DEG C, automatic drop Product is taken out to less than 60 DEG C and prepares high temperature purification by temperature；
(7) product after carbonization is placed in high temperature purification equipment, be evacuated to below 10 pas, set heating curve, used When 5h be warming up to 1050 DEG C, used time 6h is warming up to 1600 DEG C, and used time 6h is warming up to constant temperature 3 hours at 2200 DEG C, 2200 DEG C, automatically Less than 60 DEG C are cooled to, is drawn off obtaining carbon fiber hard insulation quilt primary product；
(8) by above-mentioned primary product through mechanical butt into high temperature furnace required product.
(product longitudinal direction span is too big, and is repetitive structure, therefore as shown in Figure 1 for obtained product section vertical section structure Clipped), product is bonded into an integral heat insulation heat-insulating heat-preserving material, net tire unit 3 and glue spraying by 15 layers of net tire unit stacking Layer 2 is apart from one another by arrangement, the visible longitudinal carbon fiber 4 formed by acupuncture in net tire unit 3.The non-additional protection film of the product Layer, for being used under general environment.
Embodiment 2
A kind of preparation method of the hard heat-insulated felt of low density carbon fiber, step are as follows：
(1) using the fine base carbon fibre of the polypropylene of carbon content >=92% as raw material, carbon fiber is chopped into 3-30mm, with combing Machine is combed into lousiness and net tire is made, and net tire grammes per square metre is 100g/m2, thickness 4mm, density 0.07g/cm3, carbon fiber arrangement Direction and plane where net tire are basically identical；
(2) 8 layers of net tire acupuncture are combined into a net tire unit using needle-punching method, the density of acupuncture for 15-20 pins/ cm；Needling direction is longitudinal direction, and net tire unit tiling direction is laterally, i.e., needling direction is vertical with plane where net tire unit.
(3) single or double spraying phenolic resin adhesion is carried out to net tire unit obtained above using fog spraying method Agent, glue spraying amount are 1.0kg/m2；
(4) 0.5mm thickness graphite papers are placed in bottommost, then the two-sided glue spraying of net tire unit by every 8 layers of net tire, are laminated 15 Unit, finally it is laminated 0.5mm thickness graphite papers；
(5) after hot press being preheating into 120 DEG C, the material being laminated is placed in hot press at once, is forced into pressure 5MPa, continue to raise hot press temperature to 195 DEG C, and keep after continuing 3 hours at a temperature of this, allow hot press Temperature fall to arrive Less than 100 DEG C, take out product and prepare carbonization；
(6) upper step product is placed into carbonizing apparatus, sets heating curve, used time 3h is warming up to 300 DEG C, now led to Enter argon gas protection, used time 20h is warming up to 700 DEG C, then used time 3.5h is warming up to constant temperature 8 hours at 1050 DEG C, 1050 DEG C, automatic drop Product is taken out to less than 60 DEG C and prepares high temperature purification by temperature；
(7) product after carbonization is placed in high temperature purification equipment, be evacuated to below 10 pas, set heating curve, used When 5h be warming up to 1050 DEG C, used time 6h is warming up to 1600 DEG C, and used time 6h is warming up to constant temperature 10 hours at 2200 DEG C, 2200 DEG C, from It is dynamic to be cooled to less than 60 DEG C, it is drawn off obtaining carbon fiber hard insulation quilt primary product；
(8) by above-mentioned primary product through specification product needed for mechanical butt into high temperature furnace.
Obtained product vertical section structure is as shown in Fig. 2 be 1,15 (glue spraying 2-net of layer of graphite linings successively from top to bottom Tire unit 3), glue spraying layer 2, graphite linings 1, the visible longitudinal carbon fiber 4 formed by acupuncture in net tire unit 3.The product adds Graphite paper, can be used in particular circumstances.
Embodiment 3
A kind of preparation method of the hard heat-insulated felt of low density carbon fiber, step are as follows：
(1) using the fine base carbon fibre of the polypropylene of carbon content >=92% as raw material, carbon fiber is chopped into 3-30mm, with combing Machine is combed into lousiness and net tire is made, and net tire grammes per square metre is 100g/m2, thickness 4mm, density 0.07g/cm3, carbon fiber arrangement Direction and plane where net tire are basically identical；
(2) 8 layers of net tire acupuncture are combined into a net tire unit using needle-punching method, the density of acupuncture for 10-20 pins/ cm2；Needling direction is longitudinal direction, and net tire unit tiling direction is laterally, i.e., needling direction is vertical with plane where net tire unit.
(3) single or double spraying phenolic resin adhesion is carried out to net tire unit obtained above using fog spraying method Agent, glue spraying amount are 0.8kg/m2；
(4) 6k carbon cloths are placed in bottom, then the net tire unit after a two-sided glue spraying is placed in and is laminated with it, then The 5mm thickness graphite papers of two-sided gluing is placed on it, then the net tire unit after 14 two-sided glue sprayings is placed in and is laminated with it, most The 6k carbon cloths stacking placed on it of one side gluing, injecting glue are contacted with net tire unit downwards afterwards；
(5) after hot press being preheating into 120 DEG C, the material being laminated is placed in hot press at once, is forced into pressure 3MPa, continue to raise hot press temperature to 195 DEG C, and keep after continuing 2 hours at a temperature of this, allow hot press Temperature fall to arrive Less than 100 DEG C, take out product and prepare carbonization；
(6) upper step product is placed into carbonizing apparatus, sets heating curve, used time 3h is warming up to 300 DEG C, now led to Enter argon gas protection, used time 20h is warming up to 700 DEG C, then used time 3.5h is warming up to constant temperature 3 hours at 1050 DEG C, 1050 DEG C, automatic drop Product is taken out to less than 60 DEG C and prepares high temperature purification by temperature；
(7) product after carbonization is placed in high temperature purification equipment, be evacuated to below 10 pas, set heating curve, used When 5h be warming up to 1050 DEG C, used time 6h is warming up to 1600 DEG C, and used time 6h is warming up to constant temperature 5 hours at 2200 DEG C, 2200 DEG C, automatically Less than 60 DEG C are cooled to, is drawn off obtaining carbon fiber hard insulation quilt primary product；
(8) by above-mentioned primary product through mechanical butt into high temperature furnace required product.
Obtained product vertical section structure is as shown in figure 3, its structure is from top to bottom：5,14 (glue sprayings of carbon fibre cloth layer Layer 2-net tire unit 3), glue spraying layer 2, graphite linings 1, glue spraying layer 2, net tire unit 3, glue spraying layer 2, carbon fibre cloth layer 5.In net tire The visible longitudinal carbon fiber 4 formed by acupuncture in unit 3.The product addition of graphite paper and carbon cloth, can be in Special Ring Used under border.
The thermal and insulating performance of hard heat-insulated felt made from above-mentioned 3 embodiments is tested, test result is shown in Table 1 It is shown.All experiments are carried out under the same terms, environment, body surface area.
The performance of insulation quilt is made in the embodiment 1-3 of table 1

Claims (9)

1. a kind of preparation method of the hard heat-insulated felt of low density carbon fiber, it is characterised in that step is as follows：
(1) using the carbon fiber of carbon content >=92% as raw material, carbon fiber is chopped into 3-30mm, lousiness is combed into simultaneously with carding machine Net tire is made, net tire grammes per square metre is 20-400g/m2, thickness 0.2-200mm, density 0.08-0.2g/cm3, carbon fiber arrangement side To with net tire where plane it is basically identical；
(2) 2-40 layer net tire acupunctures are combined into a net tire unit using needle-punching method, needling direction is longitudinal, net tire unit Direction tile as laterally, i.e., needling direction is vertical with plane where net tire unit, and the density of acupuncture is 2-50 pins/cm2；
(3) single or double glue spraying is entered to net tire unit obtained above using fog spraying method, glue spraying amount is 0.8- 1.2kg/m2；
(4) the net tire unit after glue spraying and net tire unit or protecting film are laminated；
(5) after hot press being preheating into 110-120 DEG C, the material being laminated is placed in hot press at once, is forced into pressure 3-5MPa, continue to raise hot press temperature to 195 DEG C, and keep after continuing 1-10 hours at a temperature of this, allow hot press to drop naturally Temperature takes out product and prepares carbonization to less than 100 DEG C；
(6) upper step product is placed into carbonizing apparatus, sets heating curve, used time 3h is warming up to 300 DEG C, is now passed through argon Gas shielded, used time 20h are warming up to 700 DEG C, then used time 3.5h is warming up to constant temperature 3-10 hours at 1050 DEG C, 1050 DEG C, automatic drop Product is taken out to less than 60 DEG C and prepares high temperature purification by temperature；
(7) product after carbonization is placed in high temperature purification equipment, be evacuated to below 10 pas, set heating curve, used time 5h 1050 DEG C are warming up to, used time 6h is warming up to 1600 DEG C, and used time 6h is warming up to constant temperature 3-10 hours at 2200 DEG C, 2200 DEG C, automatically Less than 60 DEG C are cooled to, is drawn off obtaining carbon fiber hard insulation quilt primary product；
(8) above-mentioned primary product are machined into high temperature furnace required product.
2. the preparation method of the hard heat-insulated felt of low density carbon fiber according to claim 1, it is characterised in that the step (1) carbon fiber material in, it is that viscose, pitch, polypropylene be fine, phenolic aldehyde is carbon fiber that raw material carbonization forms.
3. the preparation method of the hard heat-insulated felt of low density carbon fiber according to claim 1, it is characterised in that step (3) Described in glue be low viscosity adhesive, from the one or more in phenolic resin, furane resins or bismaleimide resin.
4. the preparation method of the hard heat-insulated felt of low density carbon fiber according to claim 1, it is characterised in that step (3) Middle to carry out the two-sided fog spraying of CNC high-pressure unit using numerical control glue sprayer, glue sprayer is provided with standby shower nozzle.
5. the preparation method of the hard heat-insulated felt of low density carbon fiber according to claim 1, it is characterised in that step (4) Middle protecting film includes 12k, 6k carbon cloth or 0.5-2mm graphite papers.
6. the preparation method of the hard heat-insulated felt of low density carbon fiber according to claim 1, it is characterised in that step (4) The mode of middle stacking includes net tire unit and is laminated with net tire unit, and the number of plies is 2-40 layers；Net tire unit with it is of the same race or not of the same race Protecting film is laminated, and the number of plies of net tire unit and protecting film is at least 1 layer.
7. the preparation method of the hard heat-insulated felt of low density carbon fiber according to claim 1, it is characterised in that step (8) In machining include butt, circle, perforate, wash thin mode.
8. the hard heat-insulated felt of low density carbon fiber being prepared by any methods describeds of claim 1-7, it is characterised in that bag Some net tire elementary layers are included, are bonded together between net tire elementary layer；The net tire elementary layer includes some net plies, net plies Between linked together by acupuncture.
9. the hard heat-insulated felt of low density carbon fiber according to claim 8, it is characterised in that the net tire elementary layer may be used also To be bonded together with protection film layer, protecting film layer number is at least 1 layer, and the net tire elementary layer and the bonding of protection film layer are arranged Row mode can be one layer and to one layer be intervally arranged or one layer to multilayer is intervally arranged or multilayer pair One layer of ground is intervally arranged or the random combine of above-mentioned three kinds of intervals arrangement mode.
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