CN105272254B - A kind of preparation method of pantograph carbon slide material - Google Patents
A kind of preparation method of pantograph carbon slide material Download PDFInfo
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Abstract
The present invention relates to carbon material field, specifically, is related to a kind of preparation method of pantograph carbon slide material.The preparation method includes kneading, once shaping, roasting, dipping and after baking；Aggregate is that 30~45nm of particle diameter is electrolysed graphene, particle diameter is 40~55nm semi-reinforcing hydrocarbon blacks and acicular petroleum coke in kneading；Binding agent is mid temperature pitch, and impregnating agent is impregnating pitch；It is preferably 35~45nm to be wherein electrolysed graphene particle diameter, more preferably 36~42nm, most preferably 40nm；The particle diameter of semi-reinforcing hydrocarbon black is preferably 50~65nm, more preferably 55~62nm, most preferably 60nm.The physical and chemical index of carbon draw runner material prepared by the present invention can match in excellence or beauty other carbonaceous materials, other alternative carbonaceous materials are used to produce pantograph carbon draw runner material, and so that its raw material sources is wide, price is low, preparation technology is relatively easy, technical difficulty is low, production cost is low, and properties of product are high.
Description
Technical field
The present invention relates to carbon material field, specifically, is related to a kind of preparation method of pantograph carbon slide material.
Background technology
Safety is that railway transportation produces eternal theme.Locomotive is most important power-equipment in railway transportation production.For
With the locomotive that quality is good, quantity is sufficient is provided, smoothly completing and transporting for transport task is ensured with good equipment quality
Production safety, it is the main task of Locomotive Overhaul work.
Electric locomotive pantograph carbon slide plate is " throat " portion that high ferro, motor-car and passenger-cargo electric locomotive provide power
Part, its major function are：Electric locomotive is directly contacted with contact line conducting wire by the topmost of pantograph on headstock, and from
Worked in right environment.Due to constantly producing friction and impact with contact line conducting wire in operation, so this part is a kind of warp
The expendable parts often changed.
Selection as the crucial component part carbon draw runner of pantograph carbon slide must have strict want to its combination property
Seek index：It is suitable resistivity and contact resistance, enough mechanical strengths, good anti-attrition and self lubricity, good resistance to
Heat, arc resistance and certain wearability, nowadays Chinese main flow carbon draw runner material there is pure carbon, metallurgical powder and metal-impregnated carbon to slide
Bar.
If the bulk density of carbon draw runner is less, purity is not high, resistivity is excessive, mechanical strength is undesirable, may be directly
Cause a series of indexs of pantograph carbon slide, and may therefore cause motorcycle safety accident.So to make pantograph carbon slide
It is it is required that up to standard, it is necessary to set about from key position, New Type of Carbon draw runner, its physics and chemistry are produced as main raw material(s) by the use of graphene is electrolysed
Index can fully meet the high standard required properties of pantograph carbon slide.
Patent application 201110004880.6 disclose it is a kind of with copper facing CNT strengthen Material for Pantograph Slide and its
Preparation method.The material contains Cu, CNTs, Ti3SiC2And TiB2Raw material, the volume ratio of four kinds of raw materials is V (Cu)：V(CNTs)：V
(Ti3SiC2)：V(TiB2)=(65~90)：(1~20)：(2~30)：(1~20).This method is：By four kinds of raw materials and the third three
Alcohol mixes and loads steel mould after toasting, and is first cold-pressed and is placed in again in the high temperature furnace of hydrogen shield atmosphere, is warming up to 700~900
DEG C, 5~30 minutes are incubated, sample is taken out afterwards and is cold-pressed again, then carry out double sintering at 800~900 DEG C, insulation 30~
60min。
Patent application 201310445254.X discloses a kind of manufacturer of fibre reinforced copper-based pantograph sliding material
Method, material are made up of copper, graphite, carbon fiber, and graphite and electrolytic copper powder are made with nano junction using mechanical alloying mode
The composite powder of structure carries out Alloying Treatment as matrix material, then by carbon fiber surface, its surface is covered 30~40 μ m-thicks
Copper coating, the carbon fiber after copper facing is cut into chunks, is then sintered together again with matrix.
In the prior art by petroleum coke, pitch coke, carbon black, sulphur, boron nitride, carbon fiber, native graphite, calcium chloride powder etc.
End is placed in mixer and is stirred, and the transformation of the way pitch progress kneading that mixed powder adds fusing in mixed powder is made
Processing, is made kneading material；Base at the beginning of carbon draw runner is made using the kneading material；After base at the beginning of carbon draw runner is cooled into room temperature, enter
Row calcination process, sintering carbon draw runner just base is made；Base at the beginning of sintering carbon draw runner is impregnated successively, drying process, produced.It is existing
Pantograph carbon draw runner and its manufacture method, the pure carbon carbon bar bulk density of production there was only 1.70g/cm between maximum3；Resistivity
≤60μΩ.m；Rupture strength >=30Mpa；Compression strength >=45Mpa；Shore hardness is between 75~78HS, and its volume is close
Degree, resistivity etc. directly affect pantograph key performance requirements.Sulphur, nitridation are added in the pantograph carbon slide of prior art
The chemicals such as boron, calcium chloride powder, say on stricti jurise and be not belonging to pure carbonaceous material；It is the bulk density of pantograph carbon slide, strong
The item index such as tool intensity and reliability is not ideal.The physical and chemical index not up to required, it is impossible to meet corresponding service life；It is former
Diversification high-endization of material, such as carbon fiber, native graphite material necessarily make the increase of its manufacturing cost.
The defects of for prior art, spy propose the present invention.
The content of the invention
The primary goal of the invention of the present invention is to propose a kind of preparation method of pantograph carbon slide material.
In order to realize the purpose of the present invention, the technical scheme that uses for：
A kind of preparation method of pantograph carbon slide material, it is characterised in that described preparation method include kneading, into
Type, once roasting, dipping and after baking；Electrolysis graphene, the particle diameter that aggregate in kneading is 30~45nm of particle diameter be 50~
70nm semi-reinforcing hydrocarbon blacks and acicular petroleum coke；Binding agent is mid temperature pitch, and impregnating agent is impregnating pitch；Wherein, it is electrolysed graphene
Particle diameter is preferably 35~45nm, more preferably 36~42nm, most preferably 40nm；The particle diameter of semi-reinforcing hydrocarbon black is preferably 40~
55nm, more preferably 45~55nm, most preferably 55nm.
The present invention the first optimal technical scheme be：The weight ratio that graphene is electrolysed in aggregate is 65~75%, half reinforcement
The weight of carbon black is 10~15% than the weight ratio for 15~20%, acicular petroleum coke.
The present invention the second optimal technical scheme be：The particle size range and content of acicular petroleum coke be：
Preferably：Weight percentage, particle size range and the content of the acicular petroleum coke are：
The present invention the 3rd optimal technical scheme be：It is electrolysed the purity 99.9%~99.99% of graphene；Semi-reinforcing hydrocarbon black
μ Ω m of resistivity 0.5~0.8, pH value 7.5~9；The real density 2.10g/cm of acicular petroleum coke3, ash ＜ 0.3%, wave
Send out part ＜ 0.5%；Binding agent is mid temperature pitch, 83~86 DEG C of the mid temperature pitch softening point, coking value >=49%；Impregnating pitch
Quinoline do not melt thing≤0.2%, 83~86 DEG C of softening point, coking value >=48%.
The present invention the 4th optimal technical scheme be：The weight of aggregate and binding agent ratio is 70~75：25~30, be preferably
70：30.
The present invention the 5th optimal technical scheme be：Kneading is divided into dry blend wet mixing, it is described it is dry-mixed be by proportioning by aggregate
Put into kneading pot, stirred 40~45 minutes with 40 revs/min, dry-mixed temperature is 120~135 DEG C；The wet mixing is that drip is mixed by
Green grass or young crops is first heated to 190~205 DEG C, preferably 200 DEG C；It is incubated and stirs 30~40 minutes, is then cooled to 135~145 DEG C, is divided to two
It is secondary be added to it is dry-mixed after aggregate in carry out the process of kneading, the weight of the mid temperature pitch added for the first time is total mid temperature pitch
70~80%, the kneading time is 15~25 minutes, the weight of second mid temperature pitch added for total mid temperature pitch 20~
30%, the kneading time is 15~25 minutes.
The present invention the 6th optimal technical scheme be：Extrusion forming is shaped to, the bulk density of the green article after shaping
Reach 1.76~1.77g/cm3。
The present invention the 7th optimal technical scheme be：The condition being once calcined is yes：It is every in 150~400 DEG C of heating zone
1.1~1.5 DEG C of hour heating, heats up 0.7~0.9 DEG C, is risen per hour at 600~900 DEG C per hour at 400~600 DEG C
1.1~1.5 DEG C of temperature；Heated up per hour at 900~1250 DEG C 2.3~3 DEG C；1.66~1.67g/cm of small product size density3。
The present invention the 8th optimal technical scheme be：Dipping is that impregnating pitch is heated into 210~300 DEG C, is preferably heated
To 210~250 DEG C, 1~2 hour is incubated, then impregnating pitch is risen again to 180~200 DEG C, the preheating temperature of pickled product during dipping
For 360~380 DEG C, vacuumize and suppress dipping；Rate of body weight gain 13~15%.
The present invention the 9th optimal technical scheme be：The time of after baking is 300~320h, the highest temperature of after baking
Spend for 750~800 DEG C, 1.77~1.78g/cm of small product size density3。
Technical scheme is made further explanation below：
The present invention proposes a kind of method that pantograph carbon slide material is prepared using pure carbon material, carbon slipper of the invention
Material has the characteristics of bulk density is larger, resistance is small, strong tool intensity is high, reliable high.Pantograph is produced using graphene is electrolysed
Carbon draw runner material is a kind of new carbonaceous product, has extraordinary physical and chemical index, although isostatic pressing formed graphite product properties
Enough meet pantograph carbon draw runner manufacturing technique requirent, but its price is very expensive, and domestic premium quality product is still in hair
The exhibition stage, and common charcoal element carbon material can not fully meet carbon draw runner physical and chemical index.The present invention by raw material, formula and
Preparation technology has carried out full and accurate exploration, and research has prepared a kind of utilize and has been electrolysed graphene production pantograph carbon draw runner material, its
Bulk density≤1.80g/cm3, resistivity is≤40 μ Ω m, and compression strength is >=40Mpa, and rupture strength is >=30Mpa, Xiao
Family name's hardness is >=60HS.The new carbonaceous material of charcoal element of the present invention can substitute it completely in terms of pantograph carbon draw runner production material
His charcoal element carbonaceous material.
By many experiments, research and analyse and produced as a trial with product, it is final to determine to be electrolysed graphite in terms of raw material selection
Alkene, semi-reinforcing hydrocarbon black, acicular petroleum coke are aggregate, and mid temperature pitch is binding agent, and impregnating agent is impregnating pitch.It is electrolysed graphene
Purity 99.9%~99.99%, particle diameter 40nm；The particle diameter of semi-reinforcing hydrocarbon black is 60nm, resistivity is less than 0.5 μ Ω m；Needle-like
The real density 2.10g/cm of petroleum coke3, ash ＜ 0.3%；83~86 DEG C of mid temperature pitch softening point, coking value >=49%；And
Impregnating pitch meets：When quinoline does not melt thing≤0.2%, 83~86 DEG C of softening point, be advantageous to obtain the higher roasting of bulk density
Product, be advantageous to improve yield rate, its physical and chemical index is met the needs of pantograph carbon draw runner.
In the preparation technology of carbon draw runner material, be formulated and the performance parameter of material had a great influence, particularly to bulk density,
The influence of resistivity, the porosity, mechanical degrees.In general, the volume that product is mentioned using relatively fine particle formula extrusion forming is close
Degree is big, the porosity is smaller, bending and compressive strength is high, and the present invention is mended in dispensing using the electrolysis graphene and half of hyperfine structure
Strong carbon black, then acicular petroleum coke crushed, is milled, sieves, little particle formula is reached, the maximum particle diameter of aggregate is less than
0.5mm.In this particle size range, the distribution of grain diameter directly affects the accumulation mode of particle, and particle packing is closer, and carbon is slided
The bulk density of strip material is bigger, mechanical strength is higher, in addition, in this particle size range, such as keeps granularity constant, particle mean size
Increase by more than one, coefficient of thermal expansion decline about 5%.The present invention is finally formulated using following aggregate through studying and test repeatedly,
The particle diameter 40nm of electrolysis graphene accounts for weight ratio as 65~75%；The particle diameter of semi-reinforcing hydrocarbon black is that 60nm accounts for weight ratio
For 15~20%；It is 10~15% that acicular petroleum coke, which accounts for weight ratio, by broken, milling, the specific grain of acicular petroleum coke of screening
Footpath matches：
0.5mm<Particle diameter≤0.330mm accounts for the 5% of acicular petroleum coke weight；
0.330mm<Particle diameter≤0.10mm accounts for the 15% of acicular petroleum coke weight；
0.010mm<Particle diameter≤0.070mm accounts for the 30% of acicular petroleum coke weight；
0<Particle diameter<0.070mm accounts for the 40% of acicular petroleum coke weight；
By such dispensing, at this moment, the particles of aggregates accumulation of different-grain diameter is more close, and the volume of carbon draw runner material is close
Degree, the porosity, bending and compressive strength and thermal coefficient of expansion can reach an extraordinary equilibrium valve, prepared carbon draw runner material
Expect that bulk density is big, the porosity is small, anti-folding and anti-pressing ability is strong, thermal coefficient of expansion is small.
The present invention has strict ratio requirement using extrusion forming mode, therefore to the dosage of binding agent mid temperature pitch,
The dosage of binding agent and the surface area of aggregate have direct relation, and the particle diameter of aggregate is small, and surface area is bigger, and consumption of binder is then got over
It is more, but consumption of binder is excessive, it is not easy during shaping compacted, thus the bulk density of product is smaller, and product easily becomes after being molded
Shape.Binding agent of the present invention is 70 with aggregate proportioning：30, aggregate and binding agent are after kneading, and obtained thickener is not substantially in group
Block, or have a little agglomerate, the higher products formed of bulk density is obtained after shaping.
The present invention during wet mixing, binding agent is added at twice it is dry-mixed after aggregate in carry out kneading, first
It is secondary to add 70~80% binding agent and aggregate bonding, because the amount of addition is few, the stickiness of mixture for accounting for total binding agent quality
Than relatively low, equal conditions mixing power effect under, can in a short time kneading it is uniform, after first time wet mixing, make feed particles
Particle diameter becomes big than more uniform, its specific surface area is diminished, then remaining binding agent is added, can in a short time by aggregate and
Binding agent uniformly mixes.Binding agent mid temperature pitch is added at twice, can both reduce time of wet mixing, reduces energy consumption, again can be with
Make thickener kneading uniform, obtain the good thickener of plasticity, be advantageous to the yield rate and physical property of green compact after raising shaping.
The purpose of roasting is to carbonize binder pitch, coke grid is formed between particles of aggregates, by varigrained bone
Material is bonded to an entirety securely.Little particle formula is cracked in follow-up heat treatment process when preparing carbon material
Probability can be big, and yield rate may be relatively low, heating curve, the duration of heat when present invention is by optimizing and improving roasting etc. because
Element, improve the coking rate of binding agent, overcome that little particle brings it is cracked, yield rate is low the problem of, to ensure product
The yield rate of overall target.
A roasting process of the invention is carried out under conditions of air is completely cut off, and maximum temperature reaches 900~1250 DEG C,
Heated up per hour 1.1~1.5 DEG C in 150~400 DEG C of heating zone, the lightweight fugitive constituent in roasting product is volatilized with slower speed
Discharge, the suffered pressure inside roasting product is smaller, more balances, and avoids crackle in temperature-rise period and produces, and lightweight
Component has sufficient time discharge product；At 400~600 DEG C, polycondensation reaction strengthens in roasting product, and coke initially forms, per small
0.7~0.9 DEG C of Shi Shengwen, is advantageous to improve the coking rate of binding agent, and carbonization at low temperature is changed into coking；At 600~900 DEG C, contracting
Poly- reaction continues to occur, the further coking of product, heats up 1.1~1.5 DEG C per hour；Heated up with slower heating rate,
Be advantageous to improve the bulk density and intensity of roasting product, and avoid during polycondensation reaction roasting product from being produced when shrinking and split
Line；At 900~1250 DEG C, heat up 2.3~3 DEG C, heated up with very fast heating rate per hour, the institutional framework of roasting product
Further densification.
The characteristic of impregnating pitch has important influence to dipping effect, is mainly manifested in asphalt viscosity, quinoline insolubles contains
In amount, coking value.Coking value is higher, and the bulk density of product and mechanical strength are bigger after roasting, and coking value is with softening point
Rise and increase, therefore using the higher coal tar pitch of softening point as binding agent, be advantageous to the bulk density of raising carbon draw runner material
And mechanical strength, but impregnating pitch softening point is higher, and relative viscosity is bigger, it is difficult to penetrates into the hole of pickled product and goes blue or green glue
Degree was both influenceed by nature, and was inversely proportional with heating-up temperature height.To improve dipping effect, the present invention one is to select softening point
It is >=48% pitch for 83~86 DEG C, coking value, second, being heated to impregnating pitch, to reduce the viscosity of impregnating pitch.
In general, after more than 200 DEG C, the light components in pitch start to volatilize, and 200~400 DEG C are the lightweights in impregnating pitch
The volatilization period of component, and with the rise of temperature, the molecular weight of the light components to be volatilized in impregnating pitch gradually increases, and waves
The gas of hair enters in the gas gas of pickled product, the infiltration of pitch is hampered, so in the prior art, impregnating pitch is heated to
Start to impregnate after 160~180 DEG C, the temperature of impregnating pitch heating is not over 200 DEG C, still, due to the carbonaceous product that need to be impregnated
Preheating temperature it is general all between 300~400 DEG C, so during dipping, still there is carbon of the light components from dipping
Evaporated in impregnating pitch in matter product, not only hamper the infiltration of impregnating pitch, many gas are also formd in pickled product
Impregnating pitch before impregnation, is first heated to 210~300 DEG C, is preferably heated to 210~250 DEG C by the aperture of body, the present invention,
So that the part light components in impregnating pitch volatilize away, the small molecule for particularly making part volatile is volatilized away, afterwards
Impregnating pitch of chatting about again cools to 180~200 DEG C and impregnated again, and at this moment, impregnating pitch still has than relatively low viscosity, compares appearance
Easily penetrate into pickled product, 360~380 DEG C of the preheating temperature of pickled product when the present invention impregnates, in dipping, due to impregnating pitch
Middle part light components volatilize away, not only increase the coking value of impregnating pitch, have also speeded up the infiltration of impregnating pitch,
And reduce the porosity in immersion oil product, the friendship fruit of dipping is good, is advantageous to improve the physical and chemical index of carbon draw runner.In dipping,
The carbonaceous product of first opposite dipping first vacuumize, and the purpose vacuumized is that the carbonaceous product that discharge need to impregnate open the intrapore gas of product,
In favor of the infiltration of impregnating pitch, after adding impregnating pitch, under the effect of the pressure, soaking clear pitch and being easier to penetrate into needs to soak
In the hole of the carbonaceous product of stain, so as to ensure rate of body weight gain；Quinoline insolubles in coal tar pitch is a kind of small particle, dipping
When quinoline insolubles in porous material surface shape thin film, hinder infiltration of the impregnating agent to porous material, therefore, present invention choosing
With the impregnating pitch of quinoline insolubles≤0.2%.
The present invention 750 DEG C of after baking, is continued to the pitch in pickled product by carrying out 300~320h to pickled product
Burnt, to improve the bulk density and mechanical strength of carbon draw runner material.
The present invention is with the acicular petroleum coke after particle diameter 40nm electrolysis graphene, particle diameter 60nm semi-reinforcing hydrocarbon black and proportioning
For aggregate, the mid temperature pitch of 83~86 DEG C of softening point, coking value >=49% is binding agent, is led to using super fine powder, little particle formula
Cross optimization and improve preparation technology, heating curve, the duration of heat when spy is by optimizing and improving roasting, and to leaching
The heating of stain pitch, warming up treatment, the physical and chemical index of the carbon draw runner material of preparation can match in excellence or beauty other carbonaceous materials, alternative
Other carbonaceous materials, for producing pantograph carbon draw runner material, so that its raw material sources is wide, price is low, preparation technology is relatively easy,
Technical difficulty is low, and production cost is low, and properties of product are high, and quality upper strata, its price is lower than other similar carbonaceous materials, commercially
Obtain great success.
The preparation method of electrolysis graphene is in the present invention：
1st, raw material：Using after-smithing petroleum coke and pitch coke as siccative, modified pitch is adhesive；After-smithing petroleum coke accounts for siccative
Weight/mass percentage composition is 85~90%, and the weight/mass percentage composition that pitch coke accounts for siccative is 10~15%；The matter of siccative and adhesive
It is 75 to measure percentage:25~80:20；The granularity of pitch coke is less than 0.075mm；
2nd, screening broken to siccative：The granularity of the after-smithing petroleum coke obtained after broken, screening is less than 1mm, wherein granularity
Weight/mass percentage composition for 1.0~0.5mm after-smithing petroleum coke is the 20~25% of total after-smithing petroleum coke, granularity be 0.5~
The weight/mass percentage composition of 0.075mm after-smithing petroleum coke is the 30~35% of total after-smithing petroleum coke, and granularity is forged less than 0.075mm's
The weight/mass percentage composition of petroleum coke is the 40~50% of total after-smithing petroleum coke afterwards；
It is dispensing, dry-mixed：The after-smithing petroleum coke after screening and pitch coke are weighed by formula to carry out as siccative, input kneading pot
Dry-mixed, the temperature of siccative is 120~130 DEG C, and the dry-mixed time is 35~45 minutes；
Wet mixing：Described wet mixing be by modified pitch with it is dry-mixed after obtained siccative in the bar that temperature is 130 DEG C~140 DEG C
Kneading is carried out under part together, obtains thickener, wherein modified pitch is added in siccative at twice carries out kneading；Time is 20~35
Minute；First time addition is the 45%~60% of total modified pitch quality, and second of addition is total modified pitch matter
The 40%~55% of amount；
Shaping：Obtained thickener is formed into bulk density under vibrating forming machine effect and is preferably greater than 1.72g/cm3Life
Base；
Once it is calcined：Maximum temperature reaches 1050 DEG C~1100 DEG C；
Dipping：Impregnation pressure is 1.80MPa~1.95MP, and the rate of body weight gain for ensureing carbon block after impregnating is more than 15%；
After baking：Roasting time is 144h~168h, and maximum temperature is 800 DEG C~850 DEG C；
Graphitization：Graphited electric power feeding time is 120~130h, and graphited maximum temperature is 2850~3000 DEG C；
Machining：The product after graphitization is processed into cuboid of the side with termination on request, termination is used for
Connect electricity.It is a kind of continuous consumption material for preparing the dilute graphite anode of electrolysis graphite.
Electrolytic tank electrolysis：Parallelepiped graphite slab is put into electrolytic cell, electric wire is connected on the termination of side, with 220VA electricity
It is electrolysed by 48 hours.Its cardinal principle is that pulsed electrode method does anode, inert electrode with high purity graphite material
Negative electrode is done, anode graphite electrode obtains energy in the presence of alternating pulsing current, when the part carbon atom on graphite electrode obtains
Energy reach when being enough to overcome graphite carbon atom Interaction Force, swash from into electrolyte, form the dilute colloidal sol of graphite.
Drying：The dilute colloidal sol of graphite is placed and dried in an oven with 300-500 DEG C of temperature.
Dry：The dilute colloidal sol of graphite after drying is dried, and it is dilute to obtain electrolysis graphite.
The embodiment of the present invention is only limitted to be explained further and illustrates the present invention, not to present disclosure structure
Into limitation.
Embodiment
Embodiment 1
A kind of preparation method of pantograph carbon slide material, including kneading, shaping, once be calcined, impregnate, after baking and
Machining；
Raw material ratio is：It is 65%, semi-reinforcing hydrocarbon black 20%, acicular petroleum coke 15% to be electrolysed graphene weight ratio；Bone
The weight ratio of material and binding agent mid temperature pitch is 70：30；
Wherein, purity 99.99%, the particle diameter 42nm of graphene are electrolysed；
The particle diameter of carbon black is 55nm, μ Ω m of resistivity 0.6, pH value 7.5~9；
The real density 2.10g/cm of acicular petroleum coke3, ash ＜ 0.3%, fugitive constituent ＜ 0.5%；
Binding agent is mid temperature pitch, 83~86 DEG C of the mid temperature pitch softening point, coking value >=49%；
The quinoline of impregnating pitch does not melt thing≤0.2%, 83~86 DEG C of softening point, coking value >=48%.
Weight percentage, the particle size range and content of acicular petroleum coke are：
Technological process is：
Kneading is divided into dry blend wet mixing, it is described it is dry-mixed be to put aggregate in kneading pot by proportioning into, with 40 revs/min of stirrings 45
The process of minute, dry-mixed temperature are 125 DEG C；The wet mixing is to mix pitch by be first heated to 200 DEG C, is incubated and stirs 40 points
Clock, is then cooled to 135 DEG C, be added at twice it is dry-mixed after aggregate in carry out kneading process, for the first time add medium temperature
The weight of pitch is the 75% of total mid temperature pitch, and the kneading time is 20 minutes, and the weight of second of mid temperature pitch added is
The 20% of total mid temperature pitch, kneading time are 15 minutes；
Extrusion forming is shaped to, the bulk density of the green article after shaping reaches 1.76~1.77g/cm3；
Once roasting is that the green article after shaping is put into roaster, under conditions of air is completely cut off, carries out hot place
The process of reason.The condition of heat treatment is：Maximum temperature reaches 900 DEG C, heats up 1.2 per hour in 150~400 DEG C of heating zone
DEG C, heat up 0.8 DEG C, heated up per hour at 600~900 DEG C 1.2 DEG C per hour at 400~600 DEG C；At 900~1250 DEG C
When heat up per hour 2.5 DEG C；Whole temperature-rise period is controlled with temperature alarming instrument, ensures the poor scope of temperature alarming instrument 5
Within DEG C, it is ensured that 1.66~1.67g/cm of small product size density3, the no crackle of product external and internal compositionses requirement；
Dipping is that impregnating pitch is first to heat into 220 DEG C, is incubated 2 hours, then impregnating pitch is risen again to 190 DEG C, is impregnated
When pickled product preheating temperature be 370 DEG C, vacuumize and suppress dipping；Rate of body weight gain 13-15%；
The time of after baking is 300h, and the maximum temperature of after baking is up to 800 DEG C, it is ensured that small product size density 1.77~
1.78g/cm3, the no crackle of product external and internal compositionses requirement；
Machining refers to the requirement chi that after baking product is processed into carbon draw runner national standard using various sawing machines
It is very little, can also it use the method for prior art to be processed.
The parameter by electric work carbon slipper being prepared is：Bulk density≤1.80g/cm3, resistivity is≤40 μ Ω
M, compression strength are >=40Mpa, and rupture strength is >=30Mpa, and Shore hardness is >=60HS.
Wherein, the preparation method for being electrolysed graphene is：
1st, raw material：Using after-smithing petroleum coke and pitch coke as siccative, modified pitch is adhesive；After-smithing petroleum coke accounts for siccative
Weight/mass percentage composition is 90%, and the weight/mass percentage composition that pitch coke accounts for siccative is 10%；The mass percent of siccative and adhesive
For 80:20；The granularity of pitch coke is less than 0.075mm；
2nd, screening broken to siccative：The granularity of the after-smithing petroleum coke obtained after broken, screening is less than 1mm, wherein granularity
Weight/mass percentage composition for 1.0~0.5mm after-smithing petroleum coke is the 25% of total after-smithing petroleum coke, granularity is 0.5~0.075mm
The weight/mass percentage composition of after-smithing petroleum coke be the 35% of total after-smithing petroleum coke, after-smithing petroleum coke of the granularity less than 0.075mm
Weight/mass percentage composition is the 40% of total after-smithing petroleum coke；
It is dispensing, dry-mixed：The after-smithing petroleum coke after screening and pitch coke are weighed by formula to carry out as siccative, input kneading pot
Dry-mixed, the temperature of siccative is 120 DEG C, and the dry-mixed time is 40 minutes；
Wet mixing：Kneading is carried out together with conditions of being 140 DEG C in temperature with the siccative obtained after dry-mixed by modified pitch, is obtained
To thickener, wherein modified pitch is added in siccative at twice carries out kneading, and the time is 30 minutes；First time addition is total
The 60% of modified pitch quality, second of addition are the 40% of total modified pitch quality；
Shaping：Obtained thickener is formed into bulk density under vibrating forming machine effect and is more than 1.72g/cm3Green compact；
Once it is calcined：The maximum temperature being once calcined reaches 1100 DEG C；
Dipping：Impregnation pressure is 1.95MPa, and the rate of body weight gain for ensureing carbon block after impregnating is more than 15%；
After baking：The roasting time of after baking is 168h, and maximum temperature is 850 DEG C；
Graphitization：Graphited electric power feeding time is 130h, and graphited maximum temperature is 3000 DEG C；
Machining：The product after graphitization is processed into cuboid of the side with termination on request, termination is used for
Connect electricity.It is a kind of continuous consumption material for preparing the dilute graphite anode of electrolysis graphite.
Electrolytic tank electrolysis：Parallelepiped graphite slab is put into electrolytic cell, electric wire is connected on the termination of side, with 220VA electricity
It is electrolysed by 48 hours.Its cardinal principle is that pulsed electrode method does anode, inert electrode with high purity graphite material
Negative electrode is done, anode graphite electrode obtains energy in the presence of alternating pulsing current, when the part carbon atom on graphite electrode obtains
Energy reach when being enough to overcome graphite carbon atom Interaction Force, swash from into electrolyte, form the dilute colloidal sol of graphite.
Drying：The dilute colloidal sol of graphite is placed and dried in an oven with 400 DEG C of temperature.
Dry：The dilute colloidal sol of graphite after drying is dried, and it is dilute to obtain electrolysis graphite.
Embodiment 2
A kind of preparation method of pantograph carbon slide material, including kneading, shaping, once be calcined, impregnate, after baking and
Machining；
It is 75%, semi-reinforcing hydrocarbon black 15%, acicular petroleum coke 10% to be electrolysed graphene weight ratio；Aggregate and binding agent medium temperature
The weight ratio of pitch is 75：25；
Raw material index and proportioning：
It is electrolysed purity 99.99%, the particle diameter 40nm of graphene；
The particle diameter of carbon black is 60nm, μ Ω m of resistivity 0.7, pH value 7.5~9；
The real density 2.10g/cm of acicular petroleum coke3, ash ＜ 0.3%, fugitive constituent ＜ 0.5%；
Binding agent is mid temperature pitch, 83~86 DEG C of the mid temperature pitch softening point, coking value >=49%；
The quinoline of impregnating pitch does not melt thing≤0.2%, 83~86 DEG C of softening point, coking value >=48%.
Weight percentage, the particle size range and content of the acicular petroleum coke are：
Weight percentage, particle size range and the content of the acicular petroleum coke are：
Technological process：
Kneading is divided into dry blend wet mixing, it is described it is dry-mixed be to put aggregate in kneading pot by proportioning into, with 40 revs/min of stirrings 45
The process of minute, dry-mixed temperature are 135 DEG C；The wet mixing is to mix pitch by be first heated to 200 DEG C, is incubated and stirs 40 points
Clock, is then cooled to 145 DEG C, be added at twice it is dry-mixed after aggregate in carry out kneading process, for the first time add medium temperature
The weight of pitch is the 80% of total mid temperature pitch, and the kneading time is 25 minutes, and the weight of second of mid temperature pitch added is
The 20% of total mid temperature pitch, kneading time are 20 minutes；
Extrusion forming is shaped to, the bulk density of the green article after shaping reaches 1.76~1.77g/cm3；
Once roasting is that the green article after shaping is put into roaster, under conditions of air is completely cut off, carries out hot place
The process of reason.The heat treatment process is：Maximum temperature reaches 900~1250 DEG C, in 150~400 DEG C of heating zone per hour
1.5 DEG C of heating, heats up 0.9 DEG C, is heated up per hour at 600~900 DEG C 1.5 DEG C per hour at 400~600 DEG C；900~
Heated up per hour at 1250 DEG C 3 DEG C；Whole temperature-rise period is controlled with temperature alarming instrument, ensures the poor scope of temperature alarming instrument
Within 5 DEG C, it is ensured that small product size density 1.67g/cm3, the no crackle of product external and internal compositionses requirement；
Dipping is that impregnating pitch is heated into 250 DEG C, is incubated 2 hours, then impregnating pitch is risen again to 200 DEG C, during dipping
The preheating temperature of pickled product is 380 DEG C, vacuumize and suppresses dipping；Rate of body weight gain 15%；
The time of after baking is 320h, and the maximum temperature of after baking is up to 822 DEG C, it is ensured that small product size density 1.78g/
cm3, the no crackle of product external and internal compositionses requirement；
Machining refers to the requirement chi that after baking product is processed into carbon draw runner national standard using various sawing machines
It is very little；
The parameter by electric work carbon slipper being prepared is：Bulk density≤1.80g/cm3, resistivity is≤40 μ Ω
M, compression strength are >=40Mpa, and rupture strength is >=30Mpa, and Shore hardness is >=60HS.
Wherein, the preparation method of graphene is electrolysed with embodiment 1.
The carbon draw runner of the present invention can also use the manufacture method of prior art to be processed.
Embodiment 3
A kind of preparation method of pantograph carbon slide material, including kneading, shaping, once be calcined, impregnate, after baking and
Machining；
It is 65%, semi-reinforcing hydrocarbon black 20%, acicular petroleum coke 15% to be electrolysed graphene weight ratio；Aggregate and binding agent medium temperature
The weight ratio of pitch is 72：253；
Raw material index and proportioning：
It is electrolysed purity 99.9%~99.99%, the particle diameter 40nm of graphene；
The particle diameter of carbon black is 60nm, μ Ω m of resistivity 0.7, pH value 7.5~9；
The real density 2.10g/cm of acicular petroleum coke3, ash ＜ 0.3%, fugitive constituent ＜ 0.5%；
Binding agent is mid temperature pitch, 83-86 DEG C of the mid temperature pitch softening point, coking value >=49%；
The quinoline of impregnating pitch does not melt thing≤0.2%, 83-86 DEG C of softening point, coking value >=48%.
Weight percentage, the particle size range and content of the acicular petroleum coke are：
Technological process：
Kneading is divided into dry blend wet mixing, it is described it is dry-mixed be to put aggregate in kneading pot by proportioning into, with 40 revs/min of stirrings 45
The process of minute, dry-mixed temperature are 120 DEG C；The wet mixing is to mix pitch by be first heated to 200 DEG C, is incubated and stirs 300 points
Clock, is then cooled to 135 DEG C, be added at twice it is dry-mixed after aggregate in carry out kneading process, for the first time add medium temperature
The weight of pitch is the 70% of total mid temperature pitch, and the kneading time is 15 minutes, and the weight of second of mid temperature pitch added is
The 30% of total mid temperature pitch, kneading time are 25 minutes；
Extrusion forming is shaped to, the bulk density of the green article after shaping reaches 1.76g/cm3；
Once roasting is that the green article after shaping is put into roaster, under conditions of air is completely cut off, carries out hot place
The process of reason.The heat treatment process is：Maximum temperature reaches 900~1250 DEG C, in 150~400 DEG C of heating zone per hour
1.1 DEG C of heating, heats up 0.7 DEG C, is heated up per hour at 600~900 DEG C 1.1 DEG C per hour at 400~600 DEG C；900~
Heated up per hour at 1250 DEG C 2.3 DEG C；Whole temperature-rise period is controlled with temperature alarming instrument, ensures the poor model of temperature alarming instrument
It is trapped among within 5 DEG C, it is ensured that small product size density 1.66g/cm3, the no crackle of product external and internal compositionses requirement；
Dipping is that impregnating pitch is first to heat into 230 DEG C, is incubated 1 hour, then impregnating pitch is risen again to 180 DEG C, is impregnated
When pickled product preheating temperature be 360 DEG C, vacuumize and suppress dipping；Rate of body weight gain 13-15%；
The time of after baking is 300h, and the maximum temperature of after baking is up to 750 DEG C, it is ensured that small product size density 1.77g/
cm3, the no crackle of product external and internal compositionses requirement；
Machining refers to the requirement chi that after baking product is processed into carbon draw runner national standard using various sawing machines
It is very little；The manufacture method of prior art can also be used to be processed.
Wherein, the preparation method of graphene is electrolysed with embodiment 1.
The parameter by electric work carbon slipper being prepared is：Bulk density≤1.80g/cm3, resistivity is≤40 μ Ω
M, compression strength are >=40Mpa, and rupture strength is >=30Mpa, and Shore hardness is >=60HS.
Although the present invention has been described above with particularity, but the invention is not restricted to this, those skilled in the art can
To be modified according to the principle of the present invention, therefore, the various modifications that all principles according to the present invention are carried out all should be understood to
Fall into protection scope of the present invention.
Experimental example 1
Being prepared according to the method for embodiment 1, difference is,
Comparative example 1：It for 0.08mm ordinary graphite carbon dust, particle diameter is 61nm semi-reinforcing hydrocarbon blacks to use particle diameter；
Comparative example 2：It for 60nm ordinary graphites carbon dust, particle diameter is 80nm semi-reinforcing hydrocarbon blacks to use particle diameter；
Comparative example 3：It for 90nm ordinary graphites carbon dust, particle diameter is 100nm semi-reinforcing hydrocarbon blacks to use particle diameter.
| Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Bulk density | 1.66g/cm3 | 1.67g/cm3 | 1.68g/cm3 |
| Resistivity | 44μΩ·m | 43μΩ·m | 43μΩ·m |
| Compression strength | 30Mpa | 31Mpa | 31Mpa |
| Rupture strength | 22Mpa | 23Mpa | 21Mpa |
| Shore hardness | 43HS | 42HS | 41HS |
Experimental example 2
Prepared according to the method for embodiment 1, difference is：
Comparative example 4：The weight that graphene is electrolysed in aggregate than the weight ratio for 50%, semi-reinforcing hydrocarbon black is 25%, needle-like
The weight ratio of petroleum coke is 25%；
Comparative example 5：The weight that graphene is electrolysed in aggregate than the weight ratio for 58%, semi-reinforcing hydrocarbon black is 22%, needle-like
The weight ratio of petroleum coke is 20%；
Comparative example 6：The weight that graphene is electrolysed in aggregate than the weight ratio for 60%, semi-reinforcing hydrocarbon black is 22%, needle-like
The weight ratio of petroleum coke is 18%.
| Comparative example 4 | Comparative example 5 | Comparative example 6 | |
| Bulk density | 1.72g/cm3 | 1.73g/cm3 | 1.72g/cm3 |
| Resistivity | 43μΩ·m | 45μΩ·m | 45μΩ·m |
| Compression strength | 37Mpa | 36Mpa | 36Mpa |
| Rupture strength | 29Mpa | 30Mpa | 29Mpa |
| Shore hardness | 51HS | 53HS | 52HS |
Experimental example 3
Prepared according to the method for embodiment 1, difference is：
Comparative example 7：The particle size range and content of acicular petroleum coke be：
Comparative example 8：The particle size range and content of acicular petroleum coke be：
Comparative example 9：The particle size range and content of acicular petroleum coke be：
| Comparative example 7 | Comparative example 8 | Comparative example 9 | |
| Bulk density | 1.74g/cm3 | 1.74g/cm3 | 1.73g/cm3 |
| Resistivity | 47μΩ·m | 45μΩ·m | 45μΩ·m |
| Compression strength | 34Mpa | 35Mpa | 35Mpa |
| Rupture strength | 25Mpa | 25Mpa | 26Mpa |
| Shore hardness | 50HS | 51HS | 49HS |
Claims (13)
- A kind of 1. preparation method of pantograph carbon slide material, it is characterised in that described preparation method include kneading, shaping, Once roasting, dipping and after baking；Electrolysis graphene, the particle diameter that aggregate in kneading is 30~45nm of particle diameter are 50~70nm Semi-reinforcing hydrocarbon black and acicular petroleum coke；Binding agent is mid temperature pitch, and impregnating agent is impregnating pitch, and kneading is divided into dry blend wet mixing, It is described it is dry-mixed be to put aggregate in kneading pot by proportioning into, with 40 revs/min stir 40~45 minutes, dry-mixed temperature be 120~135 ℃；The wet mixing is that mid temperature pitch is first heated to 190~205 DEG C, is incubated and stirs 30~40 minutes, is then cooled to 135 ~145 DEG C, be added at twice it is dry-mixed after aggregate in carry out the process of kneading, the weight of mid temperature pitch added for the first time is The 70~80% of total mid temperature pitch, kneading time are 15~25 minutes, and the weight of second of mid temperature pitch added drips for total medium temperature Blue or green 20~30%, kneading time are 15~25 minutes.
- 2. preparation method according to claim 1, it is characterised in that described electrolysis graphene particle diameter is 35~45nm.
- 3. preparation method according to claim 2, it is characterised in that described electrolysis graphene particle diameter is 36~42nm.
- 4. preparation method according to claim 3, it is characterised in that described electrolysis graphene particle diameter is 40nm.
- 5. preparation method according to claim 1, it is characterised in that the particle diameter of described semi-reinforcing hydrocarbon black is 55nm.
- 6. the preparation method of pantograph carbon slide material according to claim 1, it is characterised in that be electrolysed in the aggregate The weight of graphene than the weight for 65~75%, semi-reinforcing hydrocarbon black than the weight ratio for 15~20%, acicular petroleum coke be 10~ 15%。
- 7. the preparation method of pantograph carbon slide material according to claim 1, it is characterised in that the aggregate and bonding The weight ratio of agent is 70~75：25~30.
- 8. the preparation method of pantograph carbon slide material according to claim 7, it is characterised in that the aggregate and bonding The weight ratio of agent is 70：30.
- 9. the preparation method of pantograph carbon slide material according to claim 1, it is characterised in that described to be shaped to extrude Shaping, the bulk density of the green article after shaping reach 1.76~1.77g/cm3。
- 10. the preparation method of pantograph carbon slide material according to claim 1, it is characterised in that described to be once calcined Condition be yes：Heat up 1.1~1.5 DEG C in 150~400 DEG C of heating zone, heated up per hour at 400~600 DEG C per hour 0.7~0.9 DEG C, heated up per hour at 600~900 DEG C 1.1~1.5 DEG C；Heat up 2.3~3 per hour at 900~1250 DEG C ℃；1.66~1.67g/cm of small product size density3。
- 11. the preparation method of pantograph carbon slide material according to claim 1, it is characterised in that it is described dipping be by Impregnating pitch is heated to 210~300 DEG C, is incubated 1~2 hour, then impregnating pitch is risen again to 180~200 DEG C, impregnates during dipping The preheating temperature of product is 360~380 DEG C, vacuumize and suppresses dipping；Rate of body weight gain is 13%~15%.
- 12. the preparation method of pantograph carbon slide material according to claim 11, it is characterised in that it is described dipping be by Impregnating pitch is heated to 210~250 DEG C.
- 13. the preparation method of pantograph carbon slide material according to claim 1, it is characterised in that the after baking Time be 300~320h, the maximum temperature of after baking is 750~800 DEG C, 1.77~1.78g/cm of small product size density3。
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| CN106007717B (en) * | 2016-05-19 | 2019-03-05 | 大同新成新材料股份有限公司 | The preparation method of pantograph carbon slide graphene composite material |
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| CN111014696A (en) * | 2019-11-22 | 2020-04-17 | 大同新成新材料股份有限公司 | TiB2Method for preparing pantograph carbon slide bar material from/Cu composite material |
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| CN103387407B (en) * | 2013-07-22 | 2015-06-03 | 哈尔滨工业大学 | Preparation method for carbon/carbon-graphite composite material used for pantograph slide plate of high-speed train |
| CN104649700B (en) * | 2013-11-18 | 2017-02-15 | 苏州东南佳新材料股份有限公司 | Carbon contact strip of pantograph and manufacturing method thereof |
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