CN107556785A - A kind of preparation method of regeneration hard carbon black used for rubber reinforcement - Google Patents
A kind of preparation method of regeneration hard carbon black used for rubber reinforcement Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of regeneration hard carbon black used for rubber reinforcement, the preparation method is included using damaged tire as raw material, in the reduction furnace of oxygen free condition after heated by microwave removing gaseous products, obtained solid-state carbon black is reprocessed to the process that regeneration hard carbon black finished product is made, the microwave heating is passed through the dielectric gas that temperature is 350~700 DEG C into reduction furnace simultaneously, and the gaseous products of heated by microwave removing discharge reduction furnace with dielectric gas.The present invention is passed through reduction furnace with high-temperature medium gas, gaseous products caused by heated by microwave are departed from into rapidly material, it can prevent the tar steam in gaseous products from occurring to condense and be attached on solid-state carbon black due to the effect of high temperature, simultaneously, high-temperature medium gas can also carry gaseous products and depart from material, tar pollution thing therein is entirely prevented to impact carbon black particle, the solid carbon black particle structure for making rubber be obtained through Pintsch process is not destroyed, so as to keep the reinforcing rubber performance of solid-state carbon black.
Description
Technical field
The present invention is a kind of preparation method of regeneration hard carbon black used for rubber reinforcement, and in particular to one kind regeneration cracking black carbon
Preparation method, belong to carbon black preparing technical field.
Background technology
Carbon black is a kind of industrial carbon products being mainly made up of carbon, and purposes is quite varied, and the 90% of its total output is usual
It is added in rubber, is especially added in rubber tyre and is used as the hard carbon black of increase rubbery intensity.Mend
Strong carbon black has complex microstructure, i.e., has unique particle size, internal structure and surface texture on microcosmic,
For in theory, carbon black elementary particle is smaller, crystallite dimension is smaller, the defects of crystallite edge, lattice and unsaturated electric charge
It is more, i.e., inside it, surface microstructure it is more complicated, the surface energy and surface-active of such carbon black are higher, its add
Reinforcing property into rubber is better.The elementary particle particle diameter of usual hard carbon black exists in 11~500nm, specific surface area
31 × 103~85 × 103 ㎡/kg, such as：N330 is 26~30nm, and specific surface area is 73 × 103~85 × 103 ㎡/kg；N660
For 49~60nm, specific surface area is 31 × 103~43 × 103 ㎡/kg.
The production method of conventional carbon black is a lot, such as：Lamp black method, channel process, drum process, mixed gas method, steam stove method, Audit For Process
Deng, but only Audit For Process can particularly produce high-quality hard carbon black, such as because production kind of carbon black is more, quality is good：N330、
N660 etc., and account for more than the 95% of carbon black total output as the method mainly used at present, its yield.Audit For Process production of carbon black is
Using hydrocarbon-type oil as raw material, a kind of method of carbon black is produced with imperfect combustion through cracking, hydrocarbon-type oil is in China mainly with coal tar
Based on oil and its distillage carbolineum, and often producing 1 ton of carbon black averagely needs 1.60 ~ 1.84 tons of feedstock oils of consumption, consumes highest
Can reach 2 tons.It is possible thereby to know, in Audit For Process carbon black process, because raw materials for production are expensive, raw material and the energy disappear
Consume it is huge, not only make production of carbon black cost occupy it is high-leveled and difficult under, can also produce a large amount of carbon emissions, and caused by harmful substance in discharge
Environmental pollution.And on the other hand, theoretical proof, chemical and physical features are all highly stable at typical condition for carbon, mend
Chemical reaction can't occur during being added to rubber and finished product is made for strong carbon black or microstructure changes, and this is reinforcement
The main reason for carbon black is highly stable to rubber reinforcing property, sustained.As long as therefore it has been generally acknowledged that will can initially add
The original hard carbon black being added in rubber is kept completely separate with organic matter, with regard to that can obtain reinforcing property and original hard carbon black phase
When product.In order to economize on resources, reduce cost, the environmental pollution of reduction directly or indirectly, it is highly desirable that rubber can be reclaimed
Carbon black in glue product, and be used again, rubber system is reused in especially as hard carbon black.
But the carbon black being recovered at present, typically by rotary kiln or vacuum thermal cracking technology, crack damaged tire and obtain
Product carbon, i.e. conventional pyrolytic carbon black；The but this carbon black obtained as byproduct, caused because particle structure is destroyed
Quality is hardened, particle is thick, surface energy and surface-active are extremely low, can not be used in rubber, so as to lose economic value,
Long-term take is caused to stack place, pollution environment.Current existing regenerated carbon black method, used for conventional pyrolytic carbon black
Mechanical crushing, modification, ash disposal are graded one or more combinations in method, such as：
Chinese patent CN103265828A discloses a kind of solid phase graft-modification method for regenerating cracking black carbon（2013.08.28）,
By adding organic compound in thermal cracking carbon black caused by waste old, plastics Pintsch process, by milling equipment, make to have
Machine compound in situ is grafted to the surface of thermal cracking carbon black, obtains the regeneration cracking black carbon of solid phase graft-modification.But this processing
All carried out after conventional pyrolytic carbon black has been produced, no matter by how to handle, original hard carbon black is microcosmic unique
Particle size, internal structure, surface texture have all been not present, it is difficult to make its surface energy and surface-active reach original reinforcement
The level of carbon black, this modification conventional pyrolytic carbon black are even aided with Mechanical Crushing, and its reinforcing rubber performance boost is very
It is small.According to common technical knowledge it is known that Mechanical Crushing is difficult to make carbon black elementary particle reach this scope of 11~500nm, therefore
Carbon black particle specific surface area degradation, surface modification is carried out on the basis of specific surface area is extremely low and is also difficult to obtain notable effect
Fruit, carbon black can not be made to reach the requirement of reinforcing rubber.
Chinese patent CN103540172A discloses a kind of scrap rubber plastic products pyrolytic carbon ash disposal and is modified preparation, regeneration carbon black
Method and system（2014.01.29）, pyrolytic carbon is made using pyrolytic process in scrap rubber plastic products and is crushed, passes through soda acid
Reaction, wherein most ash conversion into soluble-salt and is removed, then is aided with modified change and is pyrolyzed carbon surface micro-chemical environment,
New binder course is formed, strengthens the adhesion between pyrolytic carbon particle and rubber, plastics.And ash disposal processing is carried out to carbon black, can have
Effect reduces ash content index in carbon black, but because Mechanical Crushing, surface modification can not lift the reinforcing rubber performance of carbon black in itself, because
Even if this is handled with reference to these methods, it can not equally recover the microcosmic unique particle size of carbon black, inside specific surface area
Structure, surface texture, surface energy and surface-active, carbon black can not be still set to reach the requirement of reinforcing rubber.
Above-mentioned processing method and this experienced traditional rotary kiln or true both for the post processing of conventional pyrolytic carbon black
The carbon black of empty thermal cracking processes, have occurred that elementary particle reaggregation, the microstructure heavy damage for being difficult to reverse, surface energy
Become extremely low with surface-active.Black rubber reinforcing property is first destroyed for this, then the processing method recovered, except increase
Outside process complexity, increase equipment and equipment investment and increase production cost, it is also possible to produce new environmental pollution, and final
To carbon black but can not much meet the requirement of reinforcing rubber, it is impossible to produce economic benefit, it is difficult to implemented and promoted.
The content of the invention
It is an object of the invention to provide a kind of preparation method of regeneration hard carbon black used for rubber reinforcement, high-temperature medium is used
Gas is passed through reduction furnace, wherein will depart from material rapidly by gaseous products caused by heated by microwave, on the one hand due to the work of high temperature
Occur to condense and be attached on solid-state carbon black, another aspect high-temperature medium gas with the tar steam that can be prevented in gaseous products
Gaseous products can be carried and depart from material rapidly, entirely prevent tar pollution thing therein to impact carbon black particle, make rubber
The solid carbon black particle structure that material obtains through Pintsch process is not destroyed, so as to keep the reinforcing rubber performance of solid-state carbon black.
The present invention is achieved through the following technical solutions：A kind of preparation method of regeneration hard carbon black used for rubber reinforcement, it is described
Preparation method is included using damaged tire as raw material, in the reduction furnace of oxygen free condition after heated by microwave removing gaseous products, will
The process of regeneration hard carbon black finished product is made in the solid-state carbon black reprocessing arrived, and the microwave heating is passed through temperature into reduction furnace simultaneously
The dielectric gas for 350~700 DEG C is spent, the gaseous products of heated by microwave removing discharge reduction furnace with dielectric gas.
The carbon black added in the damaged tire accounts for the 30~40% of damaged tire gross mass.
The damaged tire uses after being broken into block as raw material, and the damaged tire length after crushing is 20~500mm, width
For 20~500mm.
The time control of the microwave heating is in 3~40min.
The gaseous products include tar steam, hydrocarbon gas, CO, CO2And H2。
The dielectric gas by being passed through above reduction furnace, through the material in reduction furnace after carry gaseous products and formed mixed
Gas is closed, by being discharged below reduction furnace.
The dielectric gas includes N2, hydrocarbon gas, CO, CO2、H2Or the one or more in gaseous mixture.
Gaseous mixture in the dielectric gas is the gas after removing tar steam
The increment gas that gaseous mixture in the dielectric gas obtains after being recycled as dielectric gas in microwave heating process
Body is discharged as fuel gas or auxiliary gas.
The reprocessing step includes：
A, except steel wire, solid-state carbon black is sent into steel wire separator, through rolling repeatedly, sieve, after magnetic separation removal steel wire, obtained just
Hard carbon black processed；
B, homogeneous refines, and first hard carbon black processed made from step A is sent into carbon black crushes homogeneous refining system, obtains homogeneous
Refined hard carbon black；
C, pelletizing of carbon black, pelletizing of carbon black system is sent hard carbon black is refined made from step B into, it is 0.5~5mm to be processed into particle diameter
Particle, obtain regenerate hard carbon black finished product.
The present invention compared with prior art, has advantages below and beneficial effect：
（1）For the present invention during microwave heat rubber material prepares solid-state carbon black, temperature in use is 350~700 DEG C of Jie
The gaseous products such as tar steam that the organic principle in tire is transformed by matter gas, on-condensible gas depart from rapidly material, make
Tar pollution thing in gaseous products can not condense and be attached to surface of material, to carbon black grain when avoiding the traditional gum material from cracking
Influence caused by minor structure, cut-out change the carbon source of original carbon black particle particle diameter, inside and surface texture, avoided original
Carbon black particle between and carbon black particle surface form new strength carbon bond and close, maintain original carbon black to greatest extent
Microstructure, reduce the reinforcing property of original carbon black, the carbon black particle that final separation comes out is only relied on weaker Van der Waals
Power with reference to and seem very loose, it is only necessary to simple crushing is with regard to that can reach the performance of original carbon black.
（2）The present invention is a greater degree of reinforcing rubber performance for keeping solid-state carbon black, and the selection to damaged tire is also to have
It is required that, one, avoid from the very few damaged tire of content of carbon black, the damaged tire that content of carbon black is 30~40% should be selected as former
Material prepares regeneration hard carbon black, to reach regeneration hard carbon black in high yield；Two, avoid using other non-hard carbon black contents compared with
High damaged tire, such as performance tires, performance tires mainly emphasize wearability, not only added with the poor abrasion resistant carbon black of reinforcing property,
Also added with a large amount of non-carbon black filled materials, when performance tires are used to prepare regeneration hard carbon black, its reinforcing property is weak；Three, avoid
Using the sizing material damaged tire containing regeneration, such as bicycle tyre, carbon black inside one side reclaimed rubber prepare reclaimed rubber when
Time has been destroyed, and on the other hand, reclaimed rubber is mixed with other non-carbon impurities when preparing, and cycle tyre is used to prepare regeneration reinforcement
During carbon black, its reinforcing property is relatively low.
（3）In the inventive method, from the damaged tire that length is 20~500mm, width is 20~500mm, due to raw material
Broken magnitude relationship to system energy consumption, crush that its thinner energy consumption is higher, the present invention selects suitable size range, is meeting energy
On the premise of imitating Con trolling index, it can just be accomplished by existing ripe equipment, suitable industrial production.
（4）In the inventive method, microwave heating time control is in 3~40min, compared with the time 6-8 of conventional process scrap rubber
Hour shortens at least 90%, can not only reduce equipment energy consumption, moreover it is possible to reduces the possibility of tar steam pollution carbon black.Tradition is useless
In rubber processing process, the gaseous products such as tar steam typically by vacuum extract out either naturally overflow, due to handle when
Between it is longer, tar steam residence time near material is longer, can increase pollution may, be unfavorable for keep solid-state carbon black rubber
Reinforcing property.
（5）In the inventive method, dielectric gas from top to bottom through material and carries gaseous state production by being passed through above reduction furnace
After thing forms gaseous mixture, by being discharged below reduction furnace, dielectric gas upper entering and lower leaving from top to bottom can be quick through the mode of material
By pollutant（Gaseous products）Take away, extracted out using negative pressure during practical operation, natural inflow, while cavity cleaning is ensured,
The stable operation of equipment, suitable industrial production can also be maintained.
（6）The high-temperature medium gas that the present invention uses can use organic matter decomposition in the gas or rubber that will not discharge oxygen to produce
Raw on-condensible gas or the gaseous mixture of above two, gaseous mixture is recyclable to be heated and is used as dielectric gas, therefore need not
Dielectric gas constantly is passed through from the external world, production gas cost can be greatlyd save；, can be by gaseous mixture in actual mechanical process
Recycled, caused increment gas during continuous service after tar pollution thing is removed by tar cold-trap and gas purifier
Body can be used it for anything else as fuel gas or collection storage or separately by diversion three-way discharge system, can be produced additional economic benefit.
（7）The present invention by microwave heat made from solid-state carbon black through reprocess be made regeneration hard carbon black, reprocessing process
In, crush homogeneous refining system using steel wire separator, carbon black and pelletizing of carbon black system is used cooperatively successively, carbon black crushes
Homogeneous refining system can will obtain homogeneous refined hard carbon black except the first hard carbon black processed after steel wire is broken, refine and mend
The primary particle size of strong carbon black is 20~200nm, aggregate particle size is 0.2~10 μm, the refined obtained regeneration reinforcement of hard carbon black
Carbon black finished product grain size size is suitable, and during rubber is added to, good mixing effect, carbon black dispersion is good.
（8）The present invention, which prepares regeneration hard carbon black, has the advantages of cost of material is low, power consumption of polymer processing is low, the value of finished goods is high,
With higher economic value.Compared to traditional oils furnace black, its raw material（And energy consumption）Cost reduces by more than 50%；Compared to
Traditional thermal cracking carbon black, power consumption of polymer processing reduce by more than 30%, and the value of finished goods improves more than 400%.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of the present invention.
Wherein, 1-envelope gas feed arrangement, 2-reduction furnace, 3-envelope gas drawing mechanism, 4-steel wire separator, 5-charcoal
Black broken homogeneous refining system, 6-pelletizing of carbon black system, 7-microwave generator, 21-outlet fan housing, 22-tar cold-trap,
23-gas purifier, 24-circulating fan, 25-gas heating stove, 26-inlet wind cover, 27-material pipeline, 28-on
Push up mesh plate, 29-bottom mesh plate.
Embodiment
Goal of the invention, technical scheme and the beneficial effect of the present invention are described in further detail below.
It is noted that described further below is all exemplary, it is intended to which the required present invention is provided further
Bright, unless otherwise indicated, all technologies used herein and scientific terminology are with the common skill with the technical field of the invention
The identical meanings that art personnel are generally understood that.
Research is found, although hard carbon black does not change during being added to rubber and finished product is made,
During using rotary kiln or vacuum thermal cracking damaged tire, the part in organic principle can change into the steaming of coercibility tar
Vapour, carbon black particle structure can be impacted, be mainly manifested in：One, in cracking process, temperature of charge uniformity extreme difference, tar
Steam easily occurs to condense and be attached on carbon black on the relatively low carbon black of temperature nearby；Two, the neighbouring tar steam concentration of carbon black
Height, mass rate of emission is slow, rate of cleavage is slow, carbon black is polluted for a long time by a large amount of tar condensings；Three, it is attached to carbon blacksurface
Tar further is influenceed to be carbonized by high temperature, and between original carbon black particle and carbon black particle surface is formed
New carbon bond is closed, and becomes large-sized a large amount of carbon black elementary particles, surface-active structure is destroyed, particle is very thick and stiff,
For a kind of carbon black particle of reinforcing rubber poor performance, and this change is that generation carbon key combines to form when tar be carbonized
, adhesion is very powerful, and mechanical crushing or anaerobic high temperature roast are all difficult to change and reply original particle structure.
To improve the reinforcing rubber performance of regeneration carbon black, prior art is by changing traditional thermal cracking ash of carbon black or modification
Regeneration carbon black is made in processing, and the disrupted particle diameter of its carbon black particle and architectural characteristic can not be restored, even be aided with
Mechanical Crushing, its reinforcing rubber performance are still very low.Based on this case, fundamentally to solve carbon black particle structural change pair
The influence of its reinforcing rubber performance, the inventive method is started with from the preparation process of regeneration hard carbon black, according to carbon black particle structure
The principle of change, prevent its influence for causing structure to destroy from source, by keeping the microstructure of original carbon black not changed
Become, to reduce the reinforcing property of original carbon black, it is possessed the characteristic of original hard carbon black reinforcing rubber performance.
It is that technical solution of the present invention is further described below：
A kind of preparation method of regeneration hard carbon black used for rubber reinforcement, the preparation method is included using damaged tire as raw material, in nothing
The process of solid-state carbon black is made in the reduction furnace 2 of oxygen condition after heated by microwave removing gaseous products,
In above process, the carbon black added in damaged tire accounts for the 30~40% of damaged tire gross mass, is needed before use broken blocking
Shape, broken thickness are the damaged tire tyre sidewall thickness of itself, and broken length, width range are 20~500mm, are laid in reduction furnace
In 2, reduction furnace 2 is through N2, hydrocarbon gas, CO, CO2Or H2Come into operation after replacing oxygen etc. the dielectric gas that will not discharge oxygen, also
Former stove 2 is provided with microwave generator 7, microwave heating time is controlled in 3~40min using microwave hot gas joint carbon black reduction furnace.
In microwave heating process, nitrogen is heated to being passed through in reduction furnace 2 after 350~700 DEG C, dielectric gas is from top to bottom
Reduction furnace 2 is carried out in the lump through the material in reduction furnace 2 and gaseous products that wherein organic principle is transformed, and high temperature makes
Tar steam in gaseous products can not be condensed and is attached on material, gaseous products include tar steam, hydrocarbon gas,
CO、CO2And H2.Gaseous products discharge reduction furnace 2 with dielectric gas and form gaseous mixture in the lump, and the gaseous mixture is passed through except tar removing is steamed
It is also reusable after the pollutant such as vapour and mist of oil to make dielectric gas use.In actual use, add as dielectric gas in microwave
The increment gas obtained after being recycled in thermal process is discharged as fuel gas or auxiliary gas.
Above-mentioned preparation method also includes carrying out solid-state carbon black to reprocess the process that regeneration hard carbon black finished product is made, then locates
It is as follows to manage step：
A, except steel wire, solid-state carbon black made from said process is sent into steel wire separator 4, through rolling, sieving repeatedly, magnetic separation is gone
After steel wire, just hard carbon black processed is obtained；
B, homogeneous refines, and first hard carbon black processed made from step A is sent into carbon black crushes homogeneous refining system 5, obtains particle diameter one
Secondary 20~200nm of particle diameter, 0.2~10 μm of aggregate particle size homogeneous refined hard carbon black；
C, pelletizing of carbon black, hard carbon black will be refined made from step B and be sent into pelletizing of carbon black system 6, be processed into particle diameter for 0.5~
5mm particle, obtain regenerating hard carbon black finished product.
The embodiment of the explanation present invention, certainly, protection of the invention are enumerated with several exemplary embodiments below
Scope is not limited to following examples.
Embodiment 1：
The present embodiment be related to it is a kind of it is used for rubber reinforcement regeneration hard carbon black preparation method, the preparation method include using damaged tire as
Raw material, the process of solid-state carbon black, microwave heating is made after heated by microwave removing gaseous products in the reduction furnace 2 of oxygen free condition
The dielectric gas that temperature is 350 DEG C is passed through simultaneously, and the gaseous products of heated by microwave removing discharge reduction furnace 2 with dielectric gas.
In the present embodiment, the carbon black added in damaged tire accounts for the 30% of damaged tire gross mass, needs to be broken into bulk before use,
Broken thickness is the damaged tire tyre sidewall thickness of itself, and the length after crushing is 20 mm, width 20mm；Material passes through reduction furnace 2
Time control in 40min, i.e. material is by microwave heating time 40min, and microwave heating temperature is 300~330 DEG C, medium gas
Body uses CH4, gaseous products include tar steam, hydrocarbon gas, CO, CO2And H2。
Embodiment 2：
The present embodiment be related to it is a kind of it is used for rubber reinforcement regeneration hard carbon black preparation method, the preparation method include using damaged tire as
Raw material, the process of solid-state carbon black, microwave heating is made after heated by microwave removing gaseous products in the reduction furnace 2 of oxygen free condition
The dielectric gas that temperature is 700 DEG C is passed through simultaneously, and the gaseous products of heated by microwave removing discharge reduction furnace 2 with dielectric gas.
In the present embodiment, the carbon black added in damaged tire accounts for the 40% of damaged tire gross mass, needs to be broken into bulk before use,
Broken thickness is the damaged tire tyre sidewall thickness of itself, and the length after crushing is 500 mm, width 500mm；Material passes through reduction
The time control of stove 2 is in 3min, i.e. material is by microwave heating time 3min, and microwave heating temperature is 600~650 DEG C, medium
Gas uses N2, gaseous products include tar steam, hydrocarbon gas, CO, CO2And H2。
In actual mechanical process, N is passed through into reduction furnace 2 first2The air in reduction furnace 2 is replaced to reach anaerobic bar
Part, after starting microwave heating, the N of the dielectric gas that is passed through first preceding displaced air for it2, N2As Jie after being heated to 700 DEG C
Matter gas uses, N2It is passed through in reduction furnace 2 and passes through material, with the gaseous mixture that gaseous products are mixed to form by the bottom of reduction furnace 2
Discharge, the gaseous mixture is also reusable after removing tar steam to make dielectric gas use, and incoagulable gas therein will not adhere to
Polluted on carbon black, and it is not oxygenous, therefore it can be regarded a part for dielectric gas, it is allowed to be blended in system together
Make dielectric gas use.During microwave continuous heating gum material, the incoagulability gas in constantly caused gaseous products
Body, such as CH4And CO, constantly accumulation cause the gas in system increment this Partial Incremental gas occur can be by setting diversion three-way
Mode discharge, to be used as fuel gas or auxiliary gas.
Embodiment 3：
The present embodiment be related to it is a kind of it is used for rubber reinforcement regeneration hard carbon black preparation method, the preparation method include using damaged tire as
Raw material, the process of solid-state carbon black, microwave heating is made after heated by microwave removing gaseous products in the reduction furnace 2 of oxygen free condition
The dielectric gas that temperature is 500 DEG C is passed through simultaneously, and the gaseous products of heated by microwave removing discharge reduction furnace 2 with dielectric gas.
In the present embodiment, the carbon black added in damaged tire accounts for the 35% of damaged tire gross mass, needs to be broken into bulk before use,
Broken thickness is the damaged tire tyre sidewall thickness of itself, the mm of length 150, width 200mm after crushing；Material passes through reduction furnace 2
Time control in 20min, i.e. material is by microwave heating time 20min, and microwave heating temperature is 400~450 DEG C, medium gas
Body uses N2, gaseous products include tar steam, hydrocarbon gas, CO, CO2And H2。
As shown in figure 1, reduction furnace 2 using microwave hot gas joint carbon black reduction furnace, be provided with reduction furnace 2 material inlet,
Material outlet, air inlet and air outlet, material pipeline 27 is set in reduction furnace 2, air inlet is located at the top of reduction furnace 2, air outlet
Located at the bottom of reduction furnace 2.During actual use, material inlet of the damaged tire raw material through reduction furnace 2 is delivered on material pipeline 27, also
The material inlet of former stove 2 sets envelope gas feed arrangement 1, avoids damaged tire raw material while reduction furnace 2 is inside and outside to occur gas exchanges
It is laid on the foraminous conveyer of material pipeline 27.When microwave heats, N2After being heated to 500 DEG C by gas heating stove 25, by also
The air inlet of former stove 2 is sent into reduction furnace 2, from top to bottom through material and carries after gaseous products form gaseous mixture, by reduction furnace 2
Air outlet send out reduction furnace 2.
The present embodiment is connected with tar cold-trap 22, gas purifier 23 in turn in the air outlet of reduction furnace 2, and gaseous mixture is through Jiao
Gas heating stove 25 is delivered to through circulating fan 24 after oil cooling trap 22, the removing tar steam of gas purifier 23 and mist of oil, as Jie
Matter gas uses.During microwave continuous heating gum material, the incoagulable gas in constantly caused gaseous products, such as
CH4And CO, constantly accumulation cause the gas in system increment occur, this Partial Incremental gas can be by setting the side of diversion three-way
Formula is discharged, to be used as fuel gas or auxiliary gas.
Embodiment 4：
The present embodiment be related to it is a kind of it is used for rubber reinforcement regeneration hard carbon black preparation method, the preparation method include using damaged tire as
Raw material, solid-state carbon black is made after heated by microwave removing gaseous products in the reduction furnace 2 of oxygen free condition, solid-state carbon black through locating again
Reason obtains regenerating the process of hard carbon black finished product.
As shown in figure 1, reduction furnace 2 using microwave hot gas joint carbon black reduction furnace, be provided with reduction furnace 2 material inlet,
Material outlet, air inlet and air outlet, material pipeline 27 is set in reduction furnace 2, air inlet is located at the top of reduction furnace 2, air outlet
Located at the bottom of reduction furnace 2.In the present embodiment, the carbon black added in damaged tire accounts for the 33% of damaged tire gross mass, needs to crush before use
Into bulk, broken thickness is the damaged tire tyre sidewall thickness of itself, and the length after crushing is 180 mm, width 180mm, is actually made
Used time, material inlet of the damaged tire raw material through reduction furnace 2 are delivered on material pipeline 27, and the material inlet of reduction furnace 2 sets envelope gas
Feed arrangement 1, avoid that damaged tire raw material is laid in into the defeated of material pipeline 27 while reduction furnace 2 is inside and outside to occur gas exchanges
Send on guipure.It is 400~500 DEG C to control microwave heating temperature in reduction furnace 2, in microwave heating process, N2By gas heating stove
After 25 are heated to 550 DEG C, reduction furnace 2 is sent into by the air inlet of reduction furnace 2, from top to bottom through material and carries gaseous products
（Tar steam, hydrocarbon gas, CO, CO2And H2）After forming gaseous mixture, reduction furnace 2, reduction furnace are sent out by the air outlet of reduction furnace 2
2 air inlet sets inlet wind cover 26, and gas fan housing 21 is set out at the air outlet of reduction furnace 2.Air-out of the present embodiment in reduction furnace 2
Mouth is connected with tar cold-trap 22, gas purifier 23 in turn, and gaseous mixture is after tar cold-trap 22, gas purifier 23 remove tar removing
Gas heating stove 25 is delivered to through circulating fan 24, is used as dielectric gas, dielectric gas now includes N2, hydro carbons gas
Body, CO, CO2And H2.During microwave continuous heating gum material, the incoagulable gas in constantly caused gaseous products,
Such as CH4And CO, constantly accumulation cause the gas in system increment occur, this Partial Incremental gas can be by setting diversion three-way
Mode is discharged, to be used as fuel gas or auxiliary gas.
Material in 25min, i.e., is obtained by the time control of reduction furnace 2 by microwave heating time 25min, continuous operation
Solid-state carbon black the material outlet of reduction furnace 2 is delivered to by material pipeline 27, by the envelope gas drawing mechanism of the material outlet of reduction furnace 2
3 send out and are reprocessed, and in the present embodiment, reprocessing step is as follows：
A, except steel wire, solid-state carbon black is sent into steel wire separator 4, through rolling repeatedly, sieve, after magnetic separation removal steel wire, obtained
First hard carbon black processed；
B, homogeneous refines, and first hard carbon black processed made from step A is sent into carbon black crushes homogeneous refining system 5, obtains particle diameter one
Secondary particle diameter 20nm, 0.2 μm of aggregate particle size homogeneous refined hard carbon black；
C, pelletizing of carbon black, pelletizing of carbon black system 6 is sent hard carbon black is refined made from step B into, it is 0.5mm's to be processed into particle diameter
Particle, obtain regenerating hard carbon black finished product.
Embodiment 5：
The present embodiment be related to it is a kind of it is used for rubber reinforcement regeneration hard carbon black preparation method, the preparation method include using damaged tire as
Raw material, solid-state carbon black is made after heated by microwave removing gaseous products in the reduction furnace 2 of oxygen free condition, solid-state carbon black through locating again
Reason obtains regenerating the process of hard carbon black finished product.
As shown in figure 1, reduction furnace 2 using microwave hot gas joint carbon black reduction furnace, be provided with reduction furnace 2 material inlet,
Material outlet, air inlet and air outlet, material pipeline 27 is set in reduction furnace 2, air inlet is located at the top of reduction furnace 2, air outlet
Located at the bottom of reduction furnace 2.In the present embodiment, the carbon black added in damaged tire accounts for the 38% of damaged tire gross mass, needs to crush before use
Into bulk, broken thickness is the damaged tire tyre sidewall thickness of itself, and the length after crushing is 100 mm, width 300mm, is actually made
Used time, material inlet of the damaged tire raw material through reduction furnace 2 are delivered on material pipeline 27, and the material inlet of reduction furnace 2 sets envelope gas
Feed arrangement 1, avoid that damaged tire raw material is laid in into the defeated of material pipeline 27 while reduction furnace 2 is inside and outside to occur gas exchanges
Send on guipure.It is 550~590 DEG C to control microwave heating temperature in reduction furnace 2, in microwave heating process, H2By gas heating stove
After 25 are heated to 620 DEG C, reduction furnace 2 is sent into by the air inlet of reduction furnace 2, from top to bottom through material and carries gaseous products
（Tar steam, hydrocarbon gas, CO, CO2And H2）After forming gaseous mixture, reduction furnace 2, reduction furnace are sent out by the air outlet of reduction furnace 2
2 air inlet sets inlet wind cover 26, and gas fan housing 21 is set out at the air outlet of reduction furnace 2.Air-out of the present embodiment in reduction furnace 2
Mouth is connected with tar cold-trap 22, gas purifier 23 in turn, and gaseous mixture is after tar cold-trap 22, gas purifier 23 remove tar removing
Deliver to gas heating stove 25 through circulating fan 24, used as dielectric gas, dielectric gas now include hydrocarbon gas,
CO、CO2And H2.During microwave continuous heating gum material, the incoagulable gas in constantly caused gaseous products, such as
CH4And CO, constantly accumulation cause the gas in system increment occur, this Partial Incremental gas can be by setting the side of diversion three-way
Formula is discharged, to be used as fuel gas or auxiliary gas.
Material in 15min, i.e., is obtained by the time control of reduction furnace 2 by microwave heating time 15min, continuous operation
Solid-state carbon black the material outlet of reduction furnace 2 is delivered to by material pipeline 27, by the envelope gas drawing mechanism of the material outlet of reduction furnace 2
3 send out and are reprocessed, and in the present embodiment, reprocessing step is as follows：
A, except steel wire, solid-state carbon black is sent into steel wire separator 4, through rolling repeatedly, sieve, after magnetic separation removal steel wire, obtained
First hard carbon black processed；
B, homogeneous refines, and first hard carbon black processed made from step A is sent into carbon black crushes homogeneous refining system 5, obtains particle diameter one
Secondary particle diameter 150nm, 8 μm of aggregate particle size homogeneous refined hard carbon black；
C, pelletizing of carbon black, pelletizing of carbon black system 6 is sent hard carbon black is refined made from step B into, is processed into that particle diameter is 5mm
Grain, obtain regenerating hard carbon black finished product.
Embodiment 6：
The present embodiment be related to it is a kind of it is used for rubber reinforcement regeneration hard carbon black preparation method, the preparation method include using damaged tire as
Raw material, solid-state carbon black is made after heated by microwave removing gaseous products in the reduction furnace 2 of oxygen free condition, solid-state carbon black through locating again
Reason obtains regenerating the process of hard carbon black finished product.
As shown in figure 1, reduction furnace 2 using microwave hot gas joint carbon black reduction furnace, be provided with reduction furnace 2 material inlet,
Material outlet, air inlet and air outlet, material pipeline 27 is set in reduction furnace 2, air inlet is located at the top of reduction furnace 2, air outlet
Located at the bottom of reduction furnace 2.In the present embodiment, the carbon black added in damaged tire accounts for the 36% of damaged tire gross mass, needs to crush before use
Into bulk, broken thickness is the damaged tire tyre sidewall thickness of itself, and the length after crushing is 200 mm, width 300mm, is actually made
Used time, material inlet of the damaged tire raw material through reduction furnace 2 are delivered on material pipeline 27, and the material inlet of reduction furnace 2 sets envelope gas
Feed arrangement 1, avoid that damaged tire raw material is laid in into the defeated of material pipeline 27 while reduction furnace 2 is inside and outside to occur gas exchanges
Send on guipure.It is 400~450 DEG C to control microwave heating temperature in reduction furnace 2, in microwave heating process, CH4 is heated by gas
After stove 25 is heated to 480 DEG C, reduction furnace 2 is sent into by the air inlet of reduction furnace 2, from top to bottom through material and carries gaseous products
（Tar steam, hydrocarbon gas, CO, CO2And H2）After forming gaseous mixture, reduction furnace 2, reduction furnace are sent out by the air outlet of reduction furnace 2
2 air inlet sets inlet wind cover 26, and gas fan housing 21 is set out at the air outlet of reduction furnace 2.Air-out of the present embodiment in reduction furnace 2
Mouth is connected with tar cold-trap 22, gas purifier 23 in turn, and gaseous mixture is after tar cold-trap 22, gas purifier 23 remove tar removing
Gas heating stove 25 is delivered to through circulating fan 24, is used as dielectric gas, dielectric gas now includes CH4、CO、CO2、
H2With other hydrocarbon gas.During microwave continuous heating gum material, the incoagulability in constantly caused gaseous products
Gas, such as CH4And CO, constantly accumulation cause the gas in system increment occur, this Partial Incremental gas can be shunted by setting
The mode of threeway is discharged, to be used as fuel gas or auxiliary gas.
Material in 30min, i.e., is obtained by the time control of reduction furnace 2 by microwave heating time 30min, continuous operation
Solid-state carbon black the material outlet of reduction furnace 2 is delivered to by material pipeline 27, by the envelope gas drawing mechanism of the material outlet of reduction furnace 2
3 send out and are reprocessed, and in the present embodiment, reprocessing step is as follows：
A, except steel wire, solid-state carbon black is sent into steel wire separator 4, through rolling repeatedly, sieve, after magnetic separation removal steel wire, obtained
First hard carbon black processed；
B, homogeneous refines, and first hard carbon black processed made from step A is sent into carbon black crushes homogeneous refining system 5, obtains particle diameter one
Secondary particle diameter 90nm, 3 μm of aggregate particle size homogeneous refined hard carbon black；
C, pelletizing of carbon black, pelletizing of carbon black system 6 is sent hard carbon black is refined made from step B into, is processed into that particle diameter is 2mm
Grain, obtain regenerating hard carbon black finished product.
Embodiment 7：
The present embodiment be related to it is a kind of it is used for rubber reinforcement regeneration hard carbon black preparation method, the preparation method include using damaged tire as
Raw material, solid-state carbon black is made after heated by microwave removing gaseous products in the reduction furnace 2 of oxygen free condition, solid-state carbon black through locating again
Reason obtains regenerating the process of hard carbon black finished product.
As shown in figure 1, reduction furnace 2 using microwave hot gas joint carbon black reduction furnace, be provided with reduction furnace 2 material inlet,
Material outlet, air inlet and air outlet, material pipeline 27 is set in reduction furnace 2, air inlet is located at the top of reduction furnace 2, air outlet
Located at the bottom of reduction furnace 2.In the present embodiment, the carbon black added in damaged tire accounts for the 36% of damaged tire gross mass, needs to crush before use
Into bulk, broken thickness is the damaged tire tyre sidewall thickness of itself, and the length after crushing is 110mm, width 90mm, actual use
When, material inlet of the damaged tire raw material through reduction furnace 2 is delivered on material pipeline 27, and the material inlet of reduction furnace 2 sets envelope gas and entered
Expect device 1, avoid the inside and outside conveying for occurring that damaged tire raw material is laid in material pipeline 27 while gas exchanges of reduction furnace 2
On guipure.It is in 550~600 DEG C of microwave heating process to control microwave heating temperature in reduction furnace 2, and CO is added by gas heating stove 25
Heat is sent into reduction furnace 2 to after 650 DEG C by the air inlet of reduction furnace 2, from top to bottom through material and carries gaseous products（Tar
Steam, hydrocarbon gas, CO, CO2And H2）After forming gaseous mixture, reduction furnace 2 is sent out by the air outlet of reduction furnace 2, reduction furnace 2 enters
Inlet wind cover 26 is set at air port, gas fan housing 21 is set out at the air outlet of reduction furnace 2.The present embodiment reduction furnace 2 air outlet according to
Secondary to be connected with tar cold-trap 22, gas purifier 23, gaseous mixture is after tar cold-trap 22, gas purifier 23 remove tar removing through following
Ring blower fan 24 delivers to gas heating stove 25, is used as dielectric gas, and dielectric gas now includes hydrocarbon gas, CO, CO2
And H2.During microwave continuous heating gum material, the incoagulable gas in constantly caused gaseous products, such as CH4With
CO, constantly accumulation cause the gas in system increment occur, and this Partial Incremental gas can be arranged by way of setting diversion three-way
Go out, to be used as fuel gas or auxiliary gas.
Material by the time control of reduction furnace 2 in 8min, i.e., by microwave heating time 8min, what continuous operation obtained
Solid-state carbon black is delivered to the material outlet of reduction furnace 2 by material pipeline 27, by the envelope gas drawing mechanism 3 of the material outlet of reduction furnace 2
Send out and reprocessed, in the present embodiment, reprocessing step is as follows：
A, except steel wire, solid-state carbon black is sent into steel wire separator 4, through rolling repeatedly, sieve, after magnetic separation removal steel wire, obtained
First hard carbon black processed；
B, homogeneous refines, and first hard carbon black processed made from step A is sent into carbon black crushes homogeneous refining system 5, obtains particle diameter one
Secondary particle diameter 200nm, 10 μm of aggregate particle size homogeneous refined hard carbon black；
C, pelletizing of carbon black, pelletizing of carbon black system 6 is sent hard carbon black is refined made from step B into, is processed into that particle diameter is 4mm
Grain, obtain regenerating hard carbon black finished product.
Embodiment 8：
The present embodiment be related to it is a kind of it is used for rubber reinforcement regeneration hard carbon black preparation method, the preparation method include using damaged tire as
Raw material, solid-state carbon black is made after heated by microwave removing gaseous products in the reduction furnace 2 of oxygen free condition, solid-state carbon black through locating again
Reason obtains regenerating the process of hard carbon black finished product.
As shown in figure 1, reduction furnace 2 using microwave hot gas joint carbon black reduction furnace, be provided with reduction furnace 2 material inlet,
Material outlet, air inlet and air outlet, material pipeline 27 is set in reduction furnace 2, air inlet is located at the top of reduction furnace 2, air outlet
Located at the bottom of reduction furnace 2.In the present embodiment, the carbon black added in damaged tire accounts for the 40% of damaged tire gross mass, needs to crush before use
Into bulk, broken thickness is the damaged tire tyre sidewall thickness of itself, and the length after crushing is 150 mm, width 100mm, is actually made
Used time, material inlet of the damaged tire raw material through reduction furnace 2 are delivered on material pipeline 27, and the material inlet of reduction furnace 2 sets envelope gas
Feed arrangement 1, avoid that damaged tire raw material is laid in into the defeated of material pipeline 27 while reduction furnace 2 is inside and outside to occur gas exchanges
Send on guipure.It is 400~450 DEG C to control microwave heating temperature in reduction furnace 2, in microwave heating process, CO2By gas heating stove
After 25 are heated to 480 DEG C, reduction furnace 2 is sent into by the air inlet of reduction furnace 2, from top to bottom through material and carries gaseous products
（Tar steam, hydrocarbon gas, CO, CO2And H2）After forming gaseous mixture, reduction furnace 2, reduction furnace are sent out by the air outlet of reduction furnace 2
2 air inlet sets inlet wind cover 26, and gas fan housing 21 is set out at the air outlet of reduction furnace 2.Air-out of the present embodiment in reduction furnace 2
Mouth is connected with tar cold-trap 22, gas purifier 23 in turn, and gaseous mixture is after tar cold-trap 22, gas purifier 23 remove tar removing
Deliver to gas heating stove 25 through circulating fan 24, used as dielectric gas, dielectric gas now include hydrocarbon gas,
CO、CO2And H2.During microwave continuous heating gum material, the incoagulable gas in constantly caused gaseous products, such as
CH4And CO, constantly accumulation cause the gas in system increment occur, this Partial Incremental gas can be by setting the side of diversion three-way
Formula is discharged, to be used as fuel gas or auxiliary gas.
Material in 35min, i.e., is obtained by the time control of reduction furnace 2 by microwave heating time 35min, continuous operation
Solid-state carbon black the material outlet of reduction furnace 2 is delivered to by material pipeline 27, by the envelope gas drawing mechanism of the material outlet of reduction furnace 2
3 send out and are reprocessed, and in the present embodiment, reprocessing step is as follows：
A, except steel wire, solid-state carbon black is sent into steel wire separator 4, through rolling repeatedly, sieve, after magnetic separation removal steel wire, obtained
First hard carbon black processed；
B, homogeneous refines, and first hard carbon black processed made from step A is sent into carbon black crushes homogeneous refining system 5, obtains particle diameter one
Secondary particle diameter 60nm, 1.5 μm of aggregate particle size homogeneous refined hard carbon black；
C, pelletizing of carbon black, pelletizing of carbon black system 6 is sent hard carbon black is refined made from step B into, it is 2.2mm's to be processed into particle diameter
Particle, obtain regenerating hard carbon black finished product.
By the index parameter of the obtained regeneration hard carbon black finished product of above-described embodiment 4~6 compared with existing carbon black, see
Table 1.
Table 1
It is described above, only it is presently preferred embodiments of the present invention, any formal limitation is not done to the present invention, it is every according to this
Any simply modification, the equivalent variations that the technical spirit of invention is made to above example, each fall within protection scope of the present invention
Within.
Claims (10)
- A kind of 1. preparation method of regeneration hard carbon black used for rubber reinforcement, it is characterised in that：The preparation method is included with useless wheel Tire is raw material, in the reduction furnace of oxygen free condition（2）After middle heated by microwave removing gaseous products, obtained solid-state carbon black is located again The process of regeneration hard carbon black finished product is made in reason, and the microwave heating is simultaneously to reduction furnace（2）In be passed through temperature as 350~700 DEG C dielectric gas, heated by microwave removing gaseous products with dielectric gas discharge reduction furnace（2）.
- A kind of 2. preparation method of regeneration hard carbon black used for rubber reinforcement according to claim 1, it is characterised in that：It is described The carbon black added in damaged tire accounts for the 30~40% of damaged tire gross mass.
- A kind of 3. preparation method of regeneration hard carbon black used for rubber reinforcement according to claim 1, it is characterised in that：It is described Damaged tire uses after being broken into block as raw material, and the damaged tire length after crushing is 20~500mm, width is 20~500mm.
- A kind of 4. preparation method of regeneration hard carbon black used for rubber reinforcement according to claim 1, it is characterised in that：It is described The time control of microwave heating is in 3~40min.
- A kind of 5. preparation method of regeneration hard carbon black used for rubber reinforcement according to claim 1, it is characterised in that：It is described Gaseous products include tar steam, hydrocarbon gas, CO, CO2And H2。
- A kind of 6. preparation method of regeneration hard carbon black used for rubber reinforcement according to claim 1, it is characterised in that：It is described Dielectric gas is by reduction furnace（2）Top is passed through, through reduction furnace（2）Gaseous products are carried after interior material and form gaseous mixture, By reduction furnace（2）Discharge lower section.
- A kind of 7. preparation method of regeneration hard carbon black used for rubber reinforcement according to claim 6, it is characterised in that：It is described Dielectric gas includes N2, hydrocarbon gas, CO, CO2、H2Or the one or more in gaseous mixture.
- A kind of 8. preparation method of regeneration hard carbon black used for rubber reinforcement according to claim 7, it is characterised in that：It is described Gaseous mixture in dielectric gas is the gas after removing tar steam.
- A kind of 9. preparation method of regeneration hard carbon black used for rubber reinforcement according to claim 8, it is characterised in that：It is described The increment gas that gaseous mixture in dielectric gas obtains when being recycled as dielectric gas in microwave heating process is used as can Combustion gas body or auxiliary gas discharge.
- A kind of 10. preparation method of regeneration hard carbon black used for rubber reinforcement according to claim 1, it is characterised in that：Institute Stating reprocessing step includes：A, except steel wire, solid-state carbon black is sent into steel wire separator（4）, through rolling repeatedly, sieve, after magnetic separation removal steel wire, obtain To first hard carbon black processed；B, homogeneous refines, by just hard carbon black processed is sent into the broken homogeneous refining system of carbon black made from step A（5）, obtain quality Uniformly refined hard carbon black；C, pelletizing of carbon black, it send hard carbon black is refined made from step B into pelletizing of carbon black system（6）, be processed into particle diameter for 0.5~ 5mm particle, obtain regenerating hard carbon black finished product.
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| CN111690272A (en) * | 2020-06-18 | 2020-09-22 | 浙江工业大学 | Method for improving specific surface area of rubber pyrolysis carbon black by using simulated flue gas |
| CN111808446A (en) * | 2020-05-07 | 2020-10-23 | 安徽省克林泰迩再生资源科技有限公司 | Pyrolysis carbon black carbonized by high-temperature pyrolysis gas and preparation method thereof |
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| CN111808446A (en) * | 2020-05-07 | 2020-10-23 | 安徽省克林泰迩再生资源科技有限公司 | Pyrolysis carbon black carbonized by high-temperature pyrolysis gas and preparation method thereof |
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