CN105838116B - A kind of preparation method of either shallow cracking black carbon - Google Patents
A kind of preparation method of either shallow cracking black carbon Download PDFInfo
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- CN105838116B CN105838116B CN201610202259.3A CN201610202259A CN105838116B CN 105838116 B CN105838116 B CN 105838116B CN 201610202259 A CN201610202259 A CN 201610202259A CN 105838116 B CN105838116 B CN 105838116B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/482—Preparation from used rubber products, e.g. tyres
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Health & Medical Sciences (AREA)
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Abstract
The present invention relates to a kind of preparation method of either shallow cracking black carbon, this method includes the following steps:1) by waste old the spiral of 280 DEG C of room temperature and 280~350 DEG C of screw combinations extrusion device in either shallow crack；2) pyrolysis product with solvent dissolved, extract separation；3) resultant product becomes either shallow cracking black carbon after crushing, drying after extracting.Gained either shallow cracking black carbon surface has with reference to glue and zinc oxide, and can and new rubber formed high-content combination glue.Compared with prior art, the present invention prepares it is shallow split the environmental protection of carbon black process, obtained carbon black can generate strong combination with rubber, and reinforcing property is excellent, be a kind of new method that waste old recycles high value added utilization.
Description
Technical field
It is specifically a kind of that waste old is shallow the present invention relates to a kind of method of waste old high added value recycling
Pyrolysis product is spent through dissolving extractive process, the method for isolated excellent reinforcing property either shallow cracking black carbon.
Background technology
The rationalization processing of waste tire is the important topic of national economy sustainable development, and processing method mainly has：
Tyre rebuilding grinds rubber powder, landfill, thermal cracking and other methods, and wherein thermal cracking is method the most economical and environmentally friendly
One of.Waste tire rubber is exactly heated to 400 DEG C or more by thermal cracking, is heat-treated, and is decomposed into gas, pyrolysis oil, heat
Solve carbon black.
The gas and pyrolysis oil that thermal cracking generates are used generally as fuel, and the thermal cracking carbon black performance generated is bad,
It is not widely applied also.Sulfide and ash content (add in during rubber processing during mainly due to rubber thermal cracking
Zinc, silicon, calcium etc.) it sulfide (such as ZnS) can be converted into is deposited on carbon blacksurface, make the reduced performance of thermal cracking carbon black, utilize
It is worth relatively low, which also limits the development of thermal cracking process.To improve the performance of cracking black carbon, patent CN201410150841.0
A kind of preparation method of oxidation modification thermal cracking carbon black is proposed, though this method can improve performance, preparation process is cumbersome, and
Easily generate secondary pollution.Therefore, it is necessary to develop more excellent cracking technology, the performance of cracking black carbon is improved.
Low molecular gas or liquid are obtained relative to the structure of high temperature pyrolysis considerable damage rubber, the present invention proposes
The concept of either shallow cracking, i.e., by waste old at relatively mild temperature, the crosslinking side switch of considerable damage rubber is a small amount of to destroy
Major key, so as to fulfill the dissociation of rubbery network, the disengaging of rubber and carbon black detaches so as to which rubber be made to be generated with carbon black.It will be shallow
The product of cracking is spent, the processing such as dissolving extracting, ultrasound, centrifugation, drying is carried out, either shallow cracking black carbon product can be obtained, can be used
In the reinforcement of rubber material.The preparation method has the characteristics that efficient, the feature of environmental protection is good, and gained either shallow cracking black carbon has and rubber
The characteristics of cementing rubber alloy is high, reinforcing good, is a kind of new carbon of great exploitation potential.
Because either shallow pyrolysis product is sticky, it is impossible to use the crackers such as traditional retort, spiral heating conveying combination spiral shell
It is a kind of processing of high molecular material equipment for integrating the functions such as mixing, heating, transmission, reaction, devolatilization that bar, which squeezes out dispersion, non-
Often be conducive to carry out either shallow cracking to waste old, make waste old that main chain and cross-bond occur under heat, shearing, pressure effect
Fracture, the dissociation of rubber matrix and carbon black, so as to be conducive to prepare either shallow pyrolysis product.
Invention content
It is mended it is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide carbon black can be made in one kind
The preparation method of the strong either shallow cracking black carbon of epistasis energy.
The purpose of the present invention can be achieved through the following technical solutions：A kind of preparation method of either shallow cracking black carbon,
It is characterized in that, this method includes the following steps:
1) by waste old, either shallow cracks in spiral-Screw Extrusion-quick water-bath cooling combination unit, makes carbon black and rubber
Glue dissociates；
2) pyrolysis product with solvent dissolved, extract separation；
3) resultant product has the either shallow cracking black carbon with reference to glue after crushing, drying as surface after extracting.The carbon black with
Rubber can generate strong combination, and reinforcing property is excellent, can be largely used to rubber industry.
The waste old is waste tire or rubber through being ground into the micelle or pass through into one that size is 5-15 mesh
Step grinding becomes the rubber powder of 20-80 mesh.
Spiral-the Screw Extrusion-quick water-bath cooling combination unit is leading portion double helix heating conveyor, centre
The combined equipment of screw pressure extrusion device and the quick water-bath cooling device of back segment, wherein double helix heating conveyor add
The Heat transmission time is 5-15min, and temperature is -280 DEG C of room temperature；Screw pressure extrusion device finds time as 1~5min, temperature
It is 280~350 DEG C；Extrudate enters quick water-bath cooling device, and the pyrolysis product of acquisition cracks rubber to solve crosslinked either shallow.
Extracting described in step (1) is using Soxhlet extraction device, extraction times 24-48h, and dissolving pyrolysis product uses
Solvent is toluene or petrol and diesel oil.
Crushing described in step (2) is Ultrasonic Pulverization processing, sonication treatment time 0.5-1h, dry temperature for 50~
60℃。
Either shallow cracking black carbon obtained by step (3) contains with reference to glue and zinc oxide, and the thickness that wherein surface combines glue is 7-
20nm。
Double helix heating conveyor is existing spiral shell in the spiral-Screw Extrusion-quick water-bath cooling combination unit
Conveyer is revolved, there is double-spiral structure, there is automatic cleaning action, avoids gluing wall in rubber powder heating process, makes each heated zones
Temperature is respectively set as 100 DEG C, 200 DEG C, 260 DEG C, 280 DEG C.The screw pressure extrusion device is squeezed for single screw rod or twin-screw
Go out machine, canonical parameter is：Draw ratio L/D=30/1~52/1, screw speed 100-600r/min；Make each heated zones
Temperature is respectively set as 280 DEG C~350 DEG C, enters in water-bath after directly extruding and cools down.
Above-mentioned spiral heating conveying device is divided into two sections by function：First segment preheats transportation section, plays conveying compacting and adds
Thermal material；Second segment is under conditions of air is completely cut off, and by change of temperature field, shoddy is made to be warming up to 280 in 5-15min
℃.If for temperature more than 280 DEG C, spiral is easily attached blocking.
Above-mentioned Screw extruder devices are divided into four sections by function：First segment solid conveying section plays further conveying compacting
Material；Second segment is plasticized back pressure section, increases the pressure in screw rod and shearing, makes the rubber powder of heating in the effect of Strong shear and heat
Under, chain rupture cross-bond and molecular backbone make crosslinked rubber be detached with carbon black；Third section kneading block further applies shearing simultaneously
Temperature is increased, makes the abundant rupture crosslinks key of shoddy；Ranging from 280-350 DEG C of the extrusion temperature finds time as 1-5min, such as
The too low rubber matrix of fruit temperature is difficult to dissociate with carbon black, and temperature is excessively high, then rubber cracking vaporizes, and easily causes pollution and environmental protection is asked
Topic；4th section of temperature-fall period, reducing temperature prevents sizing material from oxidation even sizing material spontaneous combustion occurs.
Compared with prior art, the present invention has the advantage that：
1. different from the method for conventional pyrolytic kettle, gradually heated up using spiral, it is direct to reduce classic screw extruder
Equipment attrition caused by dry friction during extrusion on the basis of spiral heating, makes rubber high with carbon black using the shearing force of screw rod
Efficiency dissociates, and the thermomechanical shear force of screw extruder makes waste old mildly crack, and destroys cross-linked network, rubber
Separation is generated with carbon black, there is continuous environmental protection.
2. the liquid rubber obtained after either shallow cracking rubber separation can be used as the liquid rubber of high added value.
3. due to the generation that zinc sulphide product is greatly reduced in either shallow cracking process, it can fully utilize and be aoxidized in rubber
The value of zinc；There is no the cladding of the by-products such as zinc sulphide, and surface is remained with reference to plastic structure, make the benefit of the either shallow cracking black carbon
It has excellent performance by force, there is very high application value.
4. the pyrolysis product of screw extruder of the present invention is stripped separation using Soxhlet extraction device, on the one hand can improve
Separating rate and separation degree, another aspect toluene, petrol and diesel oil are stripped separation, toluene and petrol and diesel oil and cracking as solvent
Rubber solution performance in product is good, and toluene, petrol and diesel oil are cheap, convenient for being distilled to recover.
5. Ultrasonic Pulverization processing utilizes the dispersion effect of ultrasonic wave in a liquid, liquid is made to generate the effect of cavitation, so as to
The solid particles such as the carbon black in liquid are crushed, there is the features such as crush efficiency is high, easy to operate.
Description of the drawings
Fig. 1 is the transmission electron microscope photo of either shallow cracking black carbon；
Fig. 2 is the XRD analysis figure of different carbon blacks.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
A kind of preparation method of either shallow cracking black carbon, includes the following steps：
Step 1：Truck tire is crushed, obtains full tire rubber powder, grain size is 30 mesh；
Step 2：Waste rubber powder in double helix heating conveyor is gradually heated to 280 DEG C, is squeezed subsequently into screw rod
Go out either shallow cracking at 320 DEG C of machine to squeeze out 2 minutes, extrudate enters water-bath cooling, obtains either shallow cracking rubber；
Step 3：Either shallow lysate rubber with filter paper is wrapped up, is put into Soxhlet extraction device, is extracted with toluene equal solvent
48h；
Step 4：Filter paper is taken out, 1h is dried in 50 DEG C of baking oven, obtains either shallow cracking black carbon and jel product, is used
The copper mesh of 400 mesh wraps up the sample in filter paper, is put into ultrasound 1h in toluene solvant, solution is put into centrifuge, with
The rotating speed centrifugation 30min of 7000rpm, collects centrifugal sediment, is put into baking oven and dries 2h to get either shallow cracking black carbon.It is thoroughly
It is as shown in Figure 1 to penetrate electromicroscopic photograph, it can be seen that carbon blacksurface has one layer to combine glue, thickness 9.02nm.
The performance of the different black-reinforced natural rubbers (NR) of table 1.
Note：N330 is new carbon black, and CBlp is either shallow cracking black carbon, and CBp is Pintsch process carbon black.
In order to be analyzed in detail to structure in CBlp, X-ray diffraction characterization has been carried out to it, Fig. 2 N330,
The X-ray diffraction spectrogram of CBp, CBlp, peak value are the carbon black structure that 25.5 ° are crystallization or orientation.The X-ray diffraction peak value of ZnO
It is 31.80 °, 34.40 °, 36.28 °, 47.58 °, 56.62 °, 62.92 °, and the peak value of α-ZnS is 27.10 °, 28.20 °,
31.00 °, 39.20 °, 47.58 °, 51.80 °, 55.70 °, 56.62 °, 57.80 °, the peak value of β-ZnS is 28.20 °, 47.58 °,
56.62 °, there are peak value at exclusive 34.40 °, 36.28 °, 62.92 ° three of ZnO in CBlp, do not have then in CBp, therefore, in CBp
Zn elements and S elements are combined to be existed in the form of ZnS, and then that this variation does not occur in either shallow cracking black carbon, still with ZnO
Compound exists.
Embodiment 2
A kind of preparation method of either shallow cracking black carbon, includes the following steps：
Step 1：Automobile tire is crushed to the micelle for being broken into that size is 5-15 mesh, through further grinding as 20-80 mesh
Rubber powder；
Step 2：Waste rubber powder in double helix heating conveyor is gradually heated to 240 DEG C, is squeezed subsequently into screw rod
Go out machine and be warming up to either shallow cracking at 270 DEG C, extrudate enters water-bath cooling, squeezes out 2 minutes；
Step 3：Either shallow lysate rubber with filter paper is wrapped up, is put into Soxhlet extraction device, with solvent extraction for 24 hours；
Step 4：Filter paper is taken out, 0.5h is dried in 60 DEG C of baking oven, obtains either shallow cracking black carbon and jel product,
The sample in filter paper is wrapped up with the copper mesh of 400 mesh, ultrasound 0.5h in toluene solvant is put into, solution is put into centrifuge, with
The rotating speed centrifugation 30min of 7000rpm, collects centrifugal sediment, is put into baking oven and dries 2h to get either shallow cracking black carbon.
The performance of the different black-reinforced natural rubbers (NR) of table 2.
N330 is new carbon black, and CBlp is 270 DEG C of either shallow cracking black carbons, and CBp is Pintsch process carbon black.
Embodiment 3
A kind of preparation method of either shallow cracking black carbon, includes the following steps：
Step 1：Automobile tire is crushed to the micelle for being broken into that size is 5-15 mesh, through further grinding as 20-80 mesh
Rubber powder；
Step 2：Waste rubber powder in double helix heating conveyor is gradually heated to 280 DEG C, is squeezed subsequently into screw rod
Go out either shallow cracking at 350 DEG C of machine heating to squeeze out, extrudate enters water-bath cooling, and it is 2 minutes to find time；
Step 3：Either shallow lysate rubber with filter paper is wrapped up, is put into Soxhlet extraction device, with solvent extraction 36h；
Step 4：Filter paper is taken out, 1h is dried in 60 DEG C of baking oven, obtains either shallow cracking black carbon and jel product, is used
The copper mesh of 400 mesh wraps up the sample in filter paper, is put into ultrasound 0.5h in gasoline, solution is put into centrifuge, with 7000rpm
Rotating speed centrifugation 30min, collect centrifugal sediment, be put into baking oven dry 2h to get either shallow cracking black carbon.It contains with reference to glue
And zinc oxide.The thickness that surface combines glue is 7nm.
The performance of the different black-reinforced natural rubbers (NR) of table 3.
N330 is new carbon black, and CBlp is either shallow cracking black carbon, and CBp is Pintsch process carbon black.
Claims (4)
1. a kind of preparation method of either shallow cracking black carbon, which is characterized in that this method includes the following steps:
1) by waste old, either shallow cracks in spiral-Screw Extrusion-quick water-bath cooling combination unit, makes carbon black and rubber solution
From；
2) pyrolysis product with solvent dissolved, extract separation；
3) resultant product has the either shallow cracking black carbon with reference to glue after crushing, drying as surface after extracting；
Spiral-the Screw Extrusion-quick water-bath cooling combination unit is leading portion double helix heating conveyor, middle screw rod
The heating of the combined equipment of pressure extrusion device and the quick water-bath cooling device of back segment, wherein double helix heating conveyor passes
The defeated time is 5-15min, and temperature is -280 DEG C of room temperature；Screw pressure extrusion device finds time as 1~5min, and temperature is
280~350 DEG C；Extrudate enters quick water-bath cooling device, and the pyrolysis product of acquisition cracks rubber to solve crosslinked either shallow；
Either shallow cracking black carbon obtained by step 3) contains with reference to glue and zinc oxide, and the thickness that wherein surface combines glue is 7-20nm.
A kind of 2. preparation method of either shallow cracking black carbon according to claim 1, which is characterized in that the waste old
It is waste tire or rubber through being ground into micelle that size is 5-15 mesh or through further grinding as the glue of 20-80 mesh
Powder.
3. the preparation method of a kind of either shallow cracking black carbon according to claim 1, which is characterized in that described in step 2)
Extracting is using Soxhlet extraction device, and the solvent that dissolving pyrolysis product uses is toluene, petrol and diesel oil solvent.
4. the preparation method of a kind of either shallow cracking black carbon according to claim 1, which is characterized in that described in step 3)
It crushes as Ultrasonic Pulverization processing.
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| CN106751898A (en) * | 2016-12-12 | 2017-05-31 | 墨宝股份有限公司 | A kind of Black flame-retardant silicon rubber material and preparation method thereof |
| EP3599219A1 (en) * | 2018-07-27 | 2020-01-29 | Black Bear Carbon B.V. | Recovered carbon black and composite material comprising said recovered carbon black |
| CN110760204B (en) * | 2019-10-25 | 2021-05-11 | 珠海格力绿色再生资源有限公司 | System and method for reducing soot ash content of waste tire cracking carbon and recovering Zn |
| CN110804229B (en) * | 2019-11-18 | 2022-05-20 | 珠海格力绿色再生资源有限公司 | Modification method of pyrolysis carbon black and application thereof |
| CN111500092A (en) * | 2020-04-15 | 2020-08-07 | 安徽省克林泰迩再生资源科技有限公司 | Modification treatment method of waste tire cracking carbon black |
| CN115260608B (en) * | 2022-08-05 | 2024-01-12 | 四川轻化工大学 | N series rubber thermal cracking carbon black combined rubber research method |
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| US5894012A (en) * | 1993-08-19 | 1999-04-13 | Gilbert W. Denison | Method and system for recovering marketable end products from waste rubber |
| CN101418082B (en) * | 2008-11-27 | 2012-05-16 | 江苏工业学院 | Green desulfurization technique of waste rubber |
| CN101508795B (en) * | 2009-03-16 | 2011-05-11 | 江苏强维橡塑科技有限公司 | Method for desulfurization regeneration of vulcanized rubber by employing double-screw extruder |
| CN102977404B (en) * | 2012-10-29 | 2014-11-05 | 北京化工大学 | Method for continuous preparation of reclaimed rubber by using dual-band twin-screw extruder |
| CN103045283B (en) * | 2012-10-31 | 2015-06-24 | 牛晓璐 | Continuous cracking process of waste rubber and device thereof |
| CN104723476B (en) * | 2013-12-23 | 2017-08-25 | 宁夏恒源晟达橡胶制品有限公司 | A kind of method that utilization junked tire produces rubber powder |
| CN103923499B (en) * | 2014-04-15 | 2015-07-08 | 北京化工大学 | Preparation method of oxidation-modified thermal cracking carbon black |
| CN104194037B (en) * | 2014-09-05 | 2017-06-27 | 淮阴工学院 | Double screw extruder and the environmental friendly regenerated dose of method of the regenerating waste used rubber of collaboration |
| CN104845391B (en) * | 2015-04-15 | 2017-08-25 | 江阴市宝利沥青新材料有限公司 | A kind of preparation method and its usage of high durable bituminous cements |
| CN105295452A (en) * | 2015-10-28 | 2016-02-03 | 贵州安泰再生资源科技有限公司 | Method for preparing low-ash-content carbon black through waste tire |
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