CN102465376A - Preparation method of highly carbonized fiber woven filler - Google Patents
Preparation method of highly carbonized fiber woven filler Download PDFInfo
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- CN102465376A CN102465376A CN2010105355878A CN201010535587A CN102465376A CN 102465376 A CN102465376 A CN 102465376A CN 2010105355878 A CN2010105355878 A CN 2010105355878A CN 201010535587 A CN201010535587 A CN 201010535587A CN 102465376 A CN102465376 A CN 102465376A
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Abstract
The invention relates to a preparation method of highly carbonized fiber woven fillers, relating to a preparation method of woven fillers. A polyacrylonitrile fiber wire bundle is processed sequentially through constant-temperature wire discharging, multi-section pre-oxidation, medium-temperature carbonization and high-temperature carbonization in a microaerobic carbon corrosion method; wherein the temperature of the low-temperature section pre-oxidation is 238-280 DEG C, and the temperature of the medium-temperature carbonization is 900-550 DEG C; and nitrogen is adopted as a carbon wire protection gas in the microaerobic carbon corrosion method, and the temperature of the high-temperature carbonization is 1450-1700 DEG C. The prepared highly carbonized fiber woven fillers has good self-lubricating performance, high strength, high modulus, good resistance against high temperature, low temperature and corrosion and good thermal conductivity, can be used for a long time in mediums with particle fluid and in rotation of high linear speed, and can also be used to replace the existing filler products of all materials.
Description
Technical field:
The present invention relates to a kind of preparation method of braided packing, be specifically related to a kind of preparation method of high temperature cabonization fibrage filler.
Background technology:
A lot of throttlings is arranged in industrial equipment, give arranging device, like high-temperature pump, high pressure reciprocating pump, high-temperature high pressure valve etc.The working position of these devices has all required good sealing, and preventing interior media to external leakage, and the sealing of motive position is often leaked the most easily, and is particularly more obvious under the working condition of certain adverse.In commercial production, there is the accident more than 60% to leak relevant with the poorly sealed interior media that causes of equipment.Particularly at high temperature, high pressure, high rotating speed; Corrosivity waits the dynamic seal (packing) under the complex working condition condition by force; Be difficult to find a desirable filler product, guarantee our equipment high efficiency operation, satisfy the requirement of these bad working environments condition lower seals with which type of airtight and watertight padding?
Chinese patent discloses a kind of method of producing the soft graphite braided packing (Granted publication number: CN1033916C); The steps include: 1, be pressed into graphite tape with graphite worm: graphite worm wherein is to be raw material with natural scale graphite or powder China ink; After the highly acid oxidation processes made it to become compound between graphite layers, washing and drying became graphite worm through the high temperature instantaneous expansion again; It comprises upper and lower pressure roller is carried out preliminary compression moulding and carries out in the pressure roller ironed once more to the graphite tape of pre-profiling of the zone face of the graphite worm that from hopper, the falls conveyer belt through being contained in circulation; Can mix acrylic ester adhesive this moment in the graphite worm raw material; 2, give the reinforcing material kiss-coating; The shape of reinforcing material wherein can be wire or woven mesh or laminar, and reinforcing material can be selected from silk thread, wire, carbon fiber; The glue that reinforcing material is hung can adopt the acrylic acid ester water-soluble polymer; The method of reinforcing material kiss-coating is to let reinforcing material from containing two of glue to passing the kiss-coating amount easy to control like this and the uniformity the sponge roller that rolls; 3, on one side of the graphite tape of moulding compound on reinforcing material; For the reinforcing material of silk thread shape, graphite tape has obtained " reinforcement " of vertical distribution; 4, oven dry: bake out temperature is 180 ℃-260 ℃; 5. at the another side of the graphite tape that is compounded with reinforcing material, be pressed into one deck graphite worm; Before getting into this step; Very do not fit between reinforcing material and the graphite tape; Graphite worm under adding from the secondary hopper is fallen on the band that is transmitting; Through the compound again last layer graphite worm of composite press roller, it is higher to make it bond strength according to " coarse " face not bonding between reinforcing material and the graphite tape; 6, cut the graphite of moulding and the composite bed band of reinforcing material; The composite graphite band of final molding gets into the broken mechanism that is with, and cuts into needed faciola, is coiled in the drum mechanism; 7, roll or twist and close: roll sub-thread or multiply to faciola through spiral and twist and close, in this process, the heart adds tinsel or nonmetal silk thread or its combination in any therein; 8, the processing on the shaping of braiding and final filler and surface; Through twisting the fine rule twist with the fingers again through cover compile, repeat to compile, various braidings such as grid volume, punching volume and be processed into expanded graphite packing with improved flexibility, finally in addition shaping and surface treatment get product.
But use in the product and graphite braided packing now that this preparation method prepares, when high pressure, high-speed rotation, because the manufacturing technique continuity of material own is bad; Tensile strength is done not high; Be prone in the use wash away, the following life-span of high-voltage high-speed is very short, needs frequent change; It is to be checked to cause equipment often to be shut down, and normal operation is produced in influence.Also have some strength ratios material such as aramid fiber, polytetrafluoroethylene fibre etc. preferably; Itself does not have conduction, heat conductivility this type material, when under the operating mode of high pressure, high temperature, high speed, using, because the frictional heat energy that rotatablely moves and produce; Can't be conducted; Thereby can produce overheated, scaling loss, just be easy to produce dielectric leakage, usually caused the technology parking, brought a lot of losses for production economy.
Summary of the invention:
The preparation method who the purpose of this invention is to provide a kind of high carbon fibre braided packing; It solves existing in prior technology because the manufacturing technique continuity of material own is bad, and tensile strength is done not high, is prone in the use wash away; The following life-span of high-voltage high-speed is very short; Need frequent change, it is to be checked to cause equipment often to be shut down, and the problem of normal operation is produced in influence; , also solved strength ratio preferably material itself do not have conduction, heat conductivility; When under the working condition of high pressure, high temperature, high speed, using; The frictional heat energy that produces owing to rotatablely move can't be conducted, thereby can produce overheated, scaling loss, just is easy to take place dielectric leakage; Serious meeting has caused the technology parking, has brought the technical problem of a lot of losses etc. for production economy.
In order to solve the existing problem of background technology; The present invention adopts following technical scheme: its preparation method is: 1, the polyacrylonitrile fibre synnema is carried out constant temperature successively and put silk, multistage pre-oxidation, middle temperature carbonization, the rotten method protection of little oxygen carbon high temperature cabonization: oxygen 238-280 ℃ in advance of wherein low section; In the temperature of warm carbonization be 900-550 ℃: little oxygen carbon erosion method is done the carbon filament protective gas with nitrogen, and the temperature of high temperature cabonization is 1450-1700 ℃;
2, the product with a last step carries out starching, receives silk, obtains the carbon fiber synnema;
3, maceration extract proportioning: with the quasi-nano graphite microparticles, Jia Songben KT1110, KT111A solvent 7-8% mix formation impregnated graphite proportioning solution, and quasi-nano graphite microparticles quality accounts for the 11-13% of impregnated graphite proportioning solution quality;
4, flood for the first time: the fiber that carbon is good carries out preliminary treatment, before braiding, material is carried out structural filling; Be fixed on carbon fiber synnema tube on the twisted filament frame; The carbon fiber synnema is progressively passed through graphite proportioning solution impregnation; Carbon fiber synnema impregnated graphite proportioning liquid is also twisted simultaneously graphite proportioning solution is fully immersed in the space of carbon fiber synnema; Reach fully saturated, the carbon fiber synnema becomes twist 105-120 twists thread, and closes rope again.
5, adopt the temperature heating of rising progressively, rising progressively from 20 ℃ is heated to 450 ℃, and Fen Shi district temperature section is evaporated cracking.Make accurate nano-graphite micro mist in carbon fiber, progressively and progressively solidify with the temperature rising with this KT1110 of pine, KT111A binding agent; Treat that until the organic matter that immerses with graphite microparticles cracking spontaneous combustion at high temperature volatilization the major part of staying in the carbon fiber all is pure graphite microparticles to the greatest extent;
6, with the quasi-nano graphite microparticles, add this KT1110 of pine, KT111A, preparation 7-8% mixes formation double-steeping graphite proportioning solution, and the quasi-nano graphite microparticles accounts for the 11-13% of double-steeping graphite proportioning solution total amount;
7, flood for the second time: be that hole and weave pattern that braided packing interlocking interlacing becomes are filled dipping; Carbon fibre braided packing, double-steeping graphite microparticles proportioning solution are put into vacuumizing formation negative pressure impregnation in the vacuum machine, and the stain time is 70-90 minute.Take out braided packing then and be rotated electric heating drying, dipping content reaches 10-12%, last moulding check warehouse-in.
The present invention has following beneficial effect: solve existing in prior technology because the manufacturing technique continuity of material own is bad; Tensile strength is done not high; Be prone in the use wash away, the following life-span of high-voltage high-speed is very short, needs frequent change; It is to be checked to cause equipment often to be shut down, and the problem of normal operation is produced in influence; Also solved strength ratio preferably material itself do not have conduction, heat conductivility; When under the working condition of high pressure, high temperature, high speed, using; The frictional heat energy that produces owing to rotatablely move can't be conducted, thereby can produce overheated, scaling loss, just is easy to take place dielectric leakage; Serious meeting has caused the technology parking, has brought the technical problem of a lot of losses etc. for production economy.
The specific embodiment:
This specific embodiment adopts following technical scheme: its preparation method is: 1, the polyacrylonitrile fibre synnema is carried out constant temperature successively and put silk, multistage pre-oxidation, middle temperature carbonization, the rotten method protection of little oxygen carbon high temperature cabonization: wherein the pre-oxidation of low section is 238-280 ℃; In the temperature of warm carbonization be 900-550 ℃: little oxygen carbon erosion method is done the carbon filament protective gas with nitrogen, and the temperature of high temperature cabonization is 1450-1700 ℃;
2, the product with a last step carries out starching, receives silk, obtains the carbon fiber synnema;
3, maceration extract proportioning: with the quasi-nano graphite microparticles, Jia Songben KT1110, KT111A solvent 7-8% mix formation impregnated graphite proportioning solution, and quasi-nano graphite microparticles quality accounts for the 11-13% of impregnated graphite proportioning solution quality;
4, flood for the first time: the fiber that carbon is good carries out preliminary treatment, before braiding, material is carried out structural filling; Be fixed on carbon fiber synnema tube on the twisted filament frame; The carbon fiber synnema is progressively passed through graphite proportioning solution impregnation; Carbon fiber synnema impregnated graphite proportioning liquid is also twisted simultaneously graphite proportioning solution is fully immersed in the space of carbon fiber synnema; Reach fully saturated, the carbon fiber synnema becomes twist 105-120 twists thread, and closes rope again.
5, adopt the temperature heating of rising progressively, rising progressively from 20 ℃ is heated to 450 ℃, and Fen Shi district temperature section is evaporated cracking.Make accurate nano-graphite micro mist in carbon fiber, progressively and progressively solidify with the temperature rising with this KT1110 of pine, KT111A binding agent; Treat that until the organic matter that immerses with graphite microparticles cracking spontaneous combustion at high temperature volatilization the major part of staying in the carbon fiber all is pure graphite microparticles to the greatest extent;
6, with the quasi-nano graphite microparticles, add this KT1110 of pine, KT111A, preparation 7-8% mixes formation double-steeping graphite proportioning solution, and the quasi-nano graphite microparticles accounts for the 11-13% of double-steeping graphite proportioning solution total amount;
7, flood for the second time: be that hole and weave pattern that braided packing interlocking interlacing becomes are filled dipping; Carbon fibre braided packing, double-steeping graphite microparticles proportioning solution are put into vacuumizing formation negative pressure impregnation in the vacuum machine, and the stain time is 70-90 minute.Take out braided packing then and be rotated electric heating drying, dipping content reaches 10-12%, last moulding check warehouse-in.
Described little oxygen carbon erosion method is used the multilayer activated carbon in the high-carbon stove; Layer mistake falls to being distributed in the nitrogen input port in the high temperature furnace hall; And on furnace hearth wall, the feed inlet and outlet of stove hall lays active carbon plate, does carbon erosion oxygen usefulness, the polyacrylonitrile fibre synnema carries out carbonization in the stove hall.Even if the polyacrylonitrile fibre synnema has during carbonization the micro amount of oxygen molecule to get into, all by activated carbon net or active carbon plate silkworm eating away, can not relate to the harm carbon filament nearby in the stove hall.
Described carbon fiber synnema is to be formed by the carbonization of polyacrylonitrile fibre synnema.
Described bonding agent is this KT1110 of pine, KT111A solvent.
Temperature in the described step 5 is risen progressively, and being heated to be rises progressively from 20 ℃ is heated to 450 ℃ of Fen Shi district temperature section evaporation cracking; Be temperature in each warm area section respectively from 20 ℃ of temperature; Rise progressively with 43 ℃ every section and to be heated to 450 ℃ of linear velocity per minute 1-1.5 rice. the impregnated carrier in the dipping proportioning liquid; Only let graphite microparticles remain in the product. temperature control seasoning in ten districts is that bake out temperature is divided into ten dry sections, sets different temperature, carries out heat drying from low to high; It is very even that product is heated, and the impregnated carrier cracking is abundant.
Drying in the said step 7 is the rotation electrothermal drying.The benefit of rotation electrothermal drying is the accurate nano-graphite micro mist solution in the braided packing, along with the rotation of equipment, can be because of the effect of gravity, and the dirty place that is deposited in of solution, thereby non-uniform phenomenon appears in density when occur producing in batches.According to the big or small this negative pressure impregnation Rotary drying of product specification, the dipping that can circulate makes product reach best quality requirement, is formed into specification at last, just can pack and put in storage.
This specific embodiment selects the polyacrylonitrile fibre synnema to carry out continuous carbonization as carbon fibre precursor; Because it has more outstanding pre-oxidation process performance, the carbide furnace circulation heating through we make utilizes ratio of specific heat speed and calculus calculation procedure; Controlled the temperature difference in the pre-oxidation furnace accurately; Make polyacrylonitrile progressively evenly heating of temperature in stove, each heat release point can accurately be controlled, can the Yin Gaowen heat release and spontaneous combustion; The preparatory oxygen of multistage ladder type makes polyacrylonitrile molecule clasp abundant, makes the linear molecule chain be converted into heat-resisting trapezium structure.Insoluble when being allowed to condition at high temperature cabonization, do not fire, and can make the time of dehydrogenation reaction and oxidation reaction sufficient, thereby obtain the preparatory oxygen silk of 850 ℃ of high temperature cabonizations.
Carbon fibre precursor polyacrylonitrile long fiber is because climatic effect has very big impact to production technology; The needed processing parameter of the precursor of different batches is different; Indefinite parameter adjustment; Very unreliable to constant product quality, so just require carbon fibre precursor is placed in the environment of 20 ℃ of constant temperature ± 2 ℃ of relative humidity 45-50% and put silk, guaranteed the make peace stability of processing parameter of precursor performance one.
Multistage pre-oxidation is that precursor carries out cyclisation, deoxidation, three reactions of oxidation in 20-450 ℃ air dielectric; Make the linear molecule chain of polyacrylonitrile fibre be converted into heat-resisting trapezium structure; It insolublely when high temperature cabonization is not fired, keep fibre morphology, thereby obtain the high-quality carbon fiber.
Will be through the fiber after the pre-oxidation through 850 ℃ middle temperature carbonization, continuously through 1450 ℃ of high temperature cabonizations of high pure nitrogen protection, the fiber that carbonization is good like this is exactly high-quality carbon fiber again.The carbon fibre tow that carbonization is good is more fluffy, and fiber alignment is mixed and disorderly, must be through sizing technique; Soak this KT1110 of pine, KT111A solution; Mixed and disorderly fibre bundle is bound, the smooth surface that becomes, fiber alignment is orderly; Can carry out a wire drawing shaft ball of string, as the semifinished material packing warehouse-in of braided packing.
High temperature cabonization mainly is the purity that solves protective gas, the nitrogen gas purity that present conventional nitrogen making machine is produced only 9.9999, and its basic demand nitrogen gas purity is greater than 9.99999 during high temperature cabonization; Otherwise be that nitrogen does not go out qualified carbon fiber synnema, avoid micro amount of oxygen silkworm erosion carbon filament, we use outside the pure protective gas of purifier apparatus; The technical staff is also through making great efforts the little oxygen carbon erosion of innovation use method on production technology in a large number; The multilayer activated carbon has been used in design in the high-carbon stove, and layer mistake falls to being distributed in the nitrogen input port in the high temperature furnace hall, even nitrogen gas purity has trace oxygen to come in inadequately; During through the activated carbon stratum reticulare by activated carbon silkworm eating away at first; And without detriment to carbon filament itself, and on furnace hearth wall, the feed inlet and outlet of stove hall also spreads active carbon plate, not only played the effect of carbon erosion oxygen; Can also assemble heat energy and improve temperature rise and render a service, and activated carbon net and active carbon plate are changed easy to maintenance in the stove hall.Can do the carbon filament protective gas with regular grade nitrogen with little oxygen carbon erosion method, produce high performance carbon fiber and come out.
This specific embodiment adopts accurate nano-graphite micro mist and this KT1110 of pine, KT111A solvent, carries out the two step infusion processes that carbon fibre initial rinse is handled and braiding back negative pressure is filled, and makes the inner impregnated graphite micro mist of braided packing full, guarantees the compactness of product.Carbon fiber is to adopt homemade polyacrylonitrile fibre bundle; Carry out pre-oxidation and two-stage high temperature cabonization through high carbide furnace; Active carbide anaerobic protection high temperature cabonization is used in innovation, thereby produces the high carbon fibre of high-performance, high temperature resistant, high strength, heat conduction height, self-lubricating, high-modulus.
The high carbon fibre braided packing self lubricity that this specific embodiment prepares, high strength, high-modulus, high-low temperature resistant, corrosion-resistant, heat conductivility all have good performance; And in containing the medium of granule fluid and in the rotation of high linear speed, can use for a long time, can be used to replace the filler product of all various materials now, solve existing in prior technology because the manufacturing technique continuity of material own is bad; Tensile strength is done not high; Be prone in the use wash away, the following life-span of high-voltage high-speed is very short, needs frequent change; It is to be checked to cause equipment often to be shut down, and the problem of normal operation is produced in influence; Also solved strength ratio preferably material itself do not have conduction, heat conductivility; When under the working condition of high pressure, high temperature, high speed, using; The frictional heat energy that produces owing to rotatablely move can't be conducted, thereby can produce overheated, scaling loss, just is easy to take place dielectric leakage; Serious meeting has caused the technology parking, has brought the technical problem of a lot of losses etc. for production economy.
Embodiment 1: the preparation method of a kind of high carbon fibre filler of this example the steps include:
1, the polyacrylonitrile fibre synnema is carried out constant temperature successively and put silk, multistage pre-oxidation, middle temperature carbonization, little oxygen carbon erosion method protection high temperature cabonization; Wherein the low-temperature carbonization temperature is 450 ℃, and the temperature of middle temperature carbonization is 850 ℃; High temperature cabonization is 1450 ℃, and little oxygen carbon erosion method is in the high-carbon stove, to use multilayer activated carbon net, and layer mistake falls to being distributed in the oxygen input port in the high temperature furnace hall; And on furnace hearth wall; The charging and discharging mouth of stove hall is laid activated carbon, and the polyacrylonitrile fibre synnema is in the stove hall during carbonization, even if there is the micro amount of oxygen molecule to get into; All nibbled nearby, can not relate to the harm carbon filament by activated carbon mesh screen or active carbon plate.
2, the product that will go up a step carries out starching, receives silk, obtains the carbon fiber synnema.
3, maceration extract proportioning with the quasi-nano graphite microparticles, adds this KT1110 of solid content pine, KT111A solvent, forms dipping proportioning solution, and quasi-nano graphite microparticles quality accounts for 15% of impregnated graphite proportioning solution gross mass.
4, flood for the first time; The carbon fiber wire bucket is fixed on the twisted filament frame; One by one through a graphite microparticles proportioning solution impregnation, the carbon fiber synnema fully immerses in the space of carbon fiber synnema a graphite microparticles proportioning solution under the effect of torsion with carbon fiber wire; Reach fully saturated, becoming the twist up to the carbon fiber synnema is 70 twist thread and synthesize rope;
5, divide ten warm areas that temperature is risen to 450 ℃ from 20 ℃; The temperature heating of rising progressively; Make accurate nano-graphite micro mist progressively solidify with bonding agent following temperature rising in carbon fiber; Organic matter cracking at high temperature volatilization until in some immersions of graphite microparticles treats that the major part of staying in the carbon fiber all is pure graphite to the greatest extent;
6, with quasi-nano graphite powder Jia Songben KT1110, KT111A solvent, mix forming double-steeping proportioning solution, the quasi-nano graphite microparticles accounts for 15% of double-steeping graphite proportioning solution gross mass;
7, flood for the second time: be that hole and weave pattern that braided packing interlocking interlacing forms are filled dipping.With carbon fibre braided packing double-steeping graphite microparticles proportioning solution, put into vacuumizing in the vacuum machine, form negative pressure impregnation, dip time is 65 minutes.Take out braided packing then and be rotated electrothermal drying, impregnating effect reaches 11%, last moulding check warehouse-in.
Embodiment 2: a kind of preparation method of high carbon fibre braided packing the steps include:
1, the polyacrylonitrile fibre synnema is carried out constant temperature successively and put silk, multistage pre-oxidation, middle temperature carbonization, little oxygen carbon erosion method protection high temperature cabonization; The temperature of warm carbonization is 850 ℃ wherein; High temperature cabonization is 1450 ℃, and little oxygen carbon erosion method is in the high-carbon stove, to use multilayer activated carbon net, and layer mistake falls to being distributed in the oxygen input port in the high temperature furnace hall; And on furnace hearth wall; The charging and discharging mouth of stove hall is laid activated carbon, and the polyacrylonitrile fibre synnema is in the stove hall during carbonization, even if there is the micro amount of oxygen molecule to get into; All nibbled nearby, can not relate to the harm carbon filament by activated carbon mesh screen or active carbon plate.
2, the product that will go up a step carries out starching, receives silk, obtains the carbon fiber synnema.
3, Jia Songben KT1110, KT111A solvent form dipping proportioning solution, and quasi-nano graphite microparticles quality accounts for 15% of impregnated graphite proportioning solution gross mass.
4, flood for the first time; The carbon fiber wire bucket is fixed on the twisted filament frame; One by one through a schungite proportioning solution impregnation, the carbon fiber synnema fully immerses in the space of carbon fiber synnema a schungite proportioning solution under the effect of torsion with carbon fiber wire; Reach fully saturated, becoming the twist up to the carbon fiber synnema is 70 twist thread and synthesize rope;
5, divide ten warm areas that temperature is risen to 450 ℃ from 20 ℃; The temperature heating of rising progressively; Make accurate nano-graphite micro mist progressively solidify with bonding agent following temperature rising in carbon fiber; Organic matter cracking at high temperature volatilization until in some immersions of graphite treats that the major part of staying in the carbon fiber all is pure graphite to the greatest extent;
6, the quasi-nano graphite microparticles is added this KT1110 of solid content pine, KT111A solvent, mix forming double-steeping proportioning solution, the quasi-nano graphite microparticles accounts for 15% of double-steeping graphite proportioning solution gross mass;
7, flood for the second time: be that hole and weave pattern that braided packing interlocking interlacing forms are filled dipping.With carbon fibre braided packing double-steeping graphite proportioning solution, put into vacuumizing in the vacuum machine, form negative pressure impregnation, dip time is 65 minutes.Take out braided packing then and be rotated electrothermal drying, impregnating effect reaches 11%, last moulding check warehouse-in.
Embodiment 3: a kind of preparation method of carbon fibre braided packing the steps include:
1, the polyacrylonitrile fibre synnema is carried out constant temperature successively and put silk, multistage pre-oxidation, middle temperature carbonization, little oxygen carbon erosion method protection high temperature cabonization; The temperature of warm carbonization is 850 ℃ wherein; High temperature cabonization is 1400 ℃, and little oxygen carbon erosion method is in the high-carbon stove, to use multilayer activated carbon net, and layer mistake falls to being distributed in the oxygen input port in the high temperature furnace hall; And on furnace hearth wall; The charging and discharging mouth of stove hall is laid activated carbon, and the polyacrylonitrile fibre synnema is in the stove hall during carbonization, even if there is the micro amount of oxygen molecule to get into; All nibbled nearby, can not relate to the harm carbon filament by activated carbon mesh screen or active carbon plate.
2, the product that will go up a step carries out starching, receives silk, obtains the carbon fiber synnema.
3, Jia Songben KT1110, KT111A solvent form dipping proportioning solution, and quasi-nano graphite microparticles quality accounts for 15% of impregnated graphite proportioning solution gross mass.
4, flood for the first time; The carbon fiber wire bucket is fixed on the twisted filament frame; One by one through a schungite proportioning solution impregnation, the carbon fiber synnema fully immerses in the space of carbon fiber synnema a schungite proportioning solution under the effect of torsion with carbon fiber wire; Reach fully saturated, becoming the twist up to the carbon fiber synnema is 70 twist thread and break into rope;
5, divide ten warm areas that temperature is risen to 450 ℃ from 20 ℃; The temperature heating of rising progressively; Make accurate nano-graphite micro mist progressively solidify with bonding agent following temperature rising in carbon fiber; Organic matter cracking at high temperature volatilization until in some immersions of graphite treats that the major part of staying in the carbon fiber all is pure graphite to the greatest extent;
6, with quasi-nano graphite microparticles Jia Songben KT1110, KT111A solvent, mix forming double-steeping proportioning solution, the quasi-nano graphite microparticles accounts for 15% of double-steeping graphite proportioning solution gross mass;
7, flood for the second time: be that hole and weave pattern that braided packing interlocking interlacing forms are filled dipping.With carbon fibre braided packing double-steeping graphite proportioning solution, put into vacuumizing in the vacuum machine, form negative pressure impregnation, dip time is 65 minutes.Take out braided packing then and be rotated electrothermal drying, impregnating effect reaches 11%, last moulding check warehouse-in.
Claims (7)
1. the preparation method of a high carbon fibre braided packing; The preparation method who it is characterized in that it is: 1, the polyacrylonitrile fibre synnema is carried out constant temperature successively and put silk, multistage pre-oxidation, middle temperature carbonization, the rotten method protection of little oxygen carbon high temperature cabonization: wherein the pre-oxidation of low section is 238-280 ℃; In the temperature of warm carbonization be 900-550 ℃: little oxygen carbon erosion method is done the carbon filament protective gas with nitrogen, and the temperature of high temperature cabonization is 1450-1700 ℃.
2. the product with a last step carries out starching, receives silk, obtains the carbon fiber synnema.
3. maceration extract proportioning: with the quasi-nano graphite microparticles, Jia Songben KT1110, KT111A solvent 7-8% mix and form impregnated graphite proportioning solution, and quasi-nano graphite microparticles quality accounts for the 11-13% of impregnated graphite proportioning solution quality.
4. flood for the first time: the fiber that carbon is good carries out preliminary treatment, before braiding, material is carried out structural filling; Be fixed on carbon fiber synnema tube on the twisted filament frame; The carbon fiber synnema is progressively passed through graphite proportioning solution impregnation; Carbon fiber synnema impregnated graphite proportioning liquid is also twisted simultaneously graphite proportioning solution is fully immersed in the space of carbon fiber synnema; Reach fully saturated, the carbon fiber synnema becomes twist 105-120 twists thread, and closes rope again.
5. adopt the temperature heating of rising progressively, rising progressively from 20 ℃ is heated to 450 ℃, and Fen Shi district temperature section is evaporated cracking; Make accurate nano-graphite micro mist in carbon fiber, progressively and progressively solidify with the temperature rising with this KT1110 of pine, KT111A binding agent; Treat that until the organic matter that immerses with graphite microparticles cracking spontaneous combustion at high temperature volatilization the major part of staying in the carbon fiber all is pure graphite microparticles to the greatest extent.
6. with the quasi-nano graphite microparticles, add this KT1110 of pine, KT111A, preparation 7-8% mixes formation double-steeping graphite proportioning solution, and the quasi-nano graphite microparticles accounts for the 11-13% of double-steeping graphite proportioning solution total amount.
7. flood for the second time: be that hole and weave pattern that braided packing interlocking interlacing becomes are filled dipping; Carbon fibre braided packing, double-steeping graphite microparticles proportioning solution are put into vacuumizing formation negative pressure impregnation in the vacuum machine, and the stain time is 70-90 minute; Take out braided packing then and be rotated electric heating drying, dipping content reaches 10-12%, last moulding check warehouse-in.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108360147A (en) * | 2018-01-09 | 2018-08-03 | 安徽弘昌新材料有限公司 | A method of preparing the pre- oxygen felt of polyacrylonitrile |
| CN117822149A (en) * | 2024-03-06 | 2024-04-05 | 建中商云(上海)碳素工程有限公司 | Carbon fiber preoxidation equipment |
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| CN117822149A (en) * | 2024-03-06 | 2024-04-05 | 建中商云(上海)碳素工程有限公司 | Carbon fiber preoxidation equipment |
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Application publication date: 20120523 |