CN106185863A - The technique that CNT prepared by the combustible gas utilizing junked tire thermal cracking to produce - Google Patents
The technique that CNT prepared by the combustible gas utilizing junked tire thermal cracking to produce Download PDFInfo
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- CN106185863A CN106185863A CN201610527586.6A CN201610527586A CN106185863A CN 106185863 A CN106185863 A CN 106185863A CN 201610527586 A CN201610527586 A CN 201610527586A CN 106185863 A CN106185863 A CN 106185863A
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- gas
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- oil
- cnt
- separation
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Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/10—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal from rubber or rubber waste
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1003—Waste materials
Abstract
The present invention relates to the technique that CNT prepared by a kind of combustible gas utilizing junked tire thermal cracking to produce, comprise the following steps: the waste tyre particle feeding pyrolysis furnace after broken is cracked, obtain air-fuel mixture gas and solid, described air-fuel mixture gas is carried out Oil-gas Separation, described solid is carried out the separation of steel wire section and white carbon black；The fuel oil obtained after Oil-gas Separation carries out cold filtration storage, and the combustible gas obtained after Oil-gas Separation is passed through the moving bed catalyst reaction device of sealing, at catalyst LaCoO3Catalytic action under obtain CNT.The unnecessary combustible gas produced when the present invention makes full use of junked tire thermal cracking carries out the production of CNT, carbon source is provided for producing CNT continuously, and device structure is simple, low cost, course of reaction is easily controlled, yield is high, has the advantages such as energy consumption is low, safe and environment-friendly, becomes the effective way preparing CNT.
Description
Technical field
The present invention relates to the preparation technology of a kind of CNT, be specifically related to one and utilize waste tire rubber thermal cracking to produce
The technique that CNT prepared by raw combustible gas.
Background technology
CNT has good mechanical property, and CNTs tensile strength reaches 50～200GPa, is 100 times of steel, close
Degree but only has the 1/6 of steel, at least higher an order of magnitude than ordinary graphite fiber；Its elastic modelling quantity is up to 1TPa, with diamond
Elastic modelling quantity suitable, about 5 times of steel.Heat conductivity is 5 times of copper, and its electric conductivity is different according to the difference of structure, Ke Yishi
Conductor, insulator, quasiconductor, it might even be possible to be only second to superconductor.Although the structure of the structure of CNT and macromolecular material
Similar, but its structure is more more stable than macromolecular material.It it is the material with high specific strength can prepared at present.If will
Make composite with Other Engineering material for matrix and CNT, can make composite material exhibits go out good intensity, elasticity,
Fatigue resistance and isotropism, bring improvement greatly to the performance of composite.CNT shows with its special structure
Extremely strong quantum effect and peculiar physical and chemical performance are gone out, at catalysis, composite, energy storage material and microelectronic component etc.
Numerous areas shows the biggest potential application foreground.The most worldwide rise the research boom of CNT,
Domestic the most once " 863 project verification " promotes carbon nanotube technology development at home.
But up to the present, the development of CNT industry be far from originally it is intended that the fastest.Prepare carbon at present
The method of nanotube has graphite acr method, laser method, a catalystic pyrolysis (CVD) etc., but this several method to there is yield few, be difficult to
Realize industrialized production.The production of multilayer carbon nanotube, also in the most primary stage, is the assay device of hundred tonnes.Generation
In the range of boundary, presently disclosed report mainly has the commerical test process units of 6 hundred tonnes of scales in operating, is all employingization
Learn the route of vapour deposition process, but production cost is higher.Conventional green people's ecology researched and developed junked tire of economic environment Protective strategy
The unnecessary cracking combustible gas produced during thermal cracking is in outdoor sky lamp burning and exhausting to air, not only pollutes environment but also waste money
Source.
Therefore, there is further optimization demand, in this is also this technical field in the preparation technology for CNT
One of study hotspot and emphasis, the present invention is accomplished especially power and starting point place.
Summary of the invention
For the above-mentioned technical problem overcoming prior art to exist, the present inventor carried out substantial amounts of further investigation it
After, thus provide a kind of combustible gas utilizing junked tire thermal cracking to produce and prepare the technique of CNT, the present invention can
Solve junked tire cracking and produce the problem that fuel gas can not make full use of and reduce CNT production cost.
The solution of above-mentioned technical problem is achieved through the following technical solutions: a kind of utilize that junked tire thermal cracking produces can
The technique of CNT is prepared in combustion gas, comprises the following steps: cracked by the waste tyre particle feeding pyrolysis furnace after broken,
Obtain air-fuel mixture gas and solid, described air-fuel mixture gas carried out Oil-gas Separation, described solid is carried out steel wire section and
The separation of white carbon black；The fuel oil obtained after Oil-gas Separation carries out cold filtration storage, and the combustible gas obtained after Oil-gas Separation is passed through close
The moving bed catalyst reaction device of envelope, at catalyst LaCoO3Catalytic action under obtain CNT.
Preferably, in described moving bed catalyst reaction device, described LaCoO3By feeding-in solid body bucket continuously and uniformly
Cloth is spread across on the red copper conveyer belt in moving bed quartz ampoule, then enters reaction zone with red copper transmission belt, and described reaction zone is with pipe
Formula stove is thermal source, and the flat-temperature zone temperature of described tube furnace controls at 700 ± 5 DEG C, junked tire thermal cracking produce combustible gas with
Described LaCoO on red copper conveyer belt3Have an effect generation CNT, by the steering-effecting of moving bed rotating shaft, described
LaCoO3On described red copper conveyer belt after remain of a predetermined time, described LaCoO3With the CNT generated from described red copper
Deviate from conveyer belt, enter catcher.It is further preferred that described LaCoO3By described feeding-in solid body bucket with 0.25g/min
The cloth amount of spilling continuous uniform cloth be spread across on described red copper conveyer belt.Further preferred, described red copper conveyer belt is with 20mm/min
Speed move into described reaction zone.It is further preferred that the external diameter of described moving bed quartz ampoule is 90mm, a length of
2000mm, the external diameter of described tube furnace is 100mm, a length of 1000mm, a length of 600mm of the flat-temperature zone of described tube furnace.
Preferably, the temperature of described cracking is 390 DEG C～420 DEG C, and the time is 25～35 minutes.It is further preferred that institute
The temperature stating cracking is 400 DEG C, and the time is 30 minutes.
Preferably, before carrying out described cracking, junked tire has first carried out pretreatment, and the process of described pretreatment is such as
Under: carry out washing with removal of contamination by the junked tire of recovery, then junked tire is sent crusher in crushing become footpath grain be 20～
The granule of 30 mm in sizes.
Preferably, the process that described air-fuel mixture gas carries out Oil-gas Separation is as follows: air-fuel mixture gas sends into cooling point
Carrying out Oil-gas Separation from tower, cool down, with cooling water, the air-fuel mixture gas entered in refrigerated separation tower, combustible gas is from cold
But escape above knockout tower, gather condensation in the bottom of refrigerated separation tower and form fuel oil, after described fuel oil is carried out filter pressing
Store.
Preferably, to carry out separating the process of steel wire section and white carbon black as follows for described solid: after described solid is come out of the stove, first by cold
But auger cools down, and utilizes separation screening auger steel wire section to be separated with white carbon black simultaneously, after the steel wire section after separation is cleaned
Recycling, white carbon black is packed after sending into flour mill pulverizing.
Compared with prior art, beneficial effects of the present invention is as follows: the present invention is on the basis of moving bed catalytic reaction technique
On, combining junked tire pyrolysis technology dexterously, the combustible gas produced when utilizing junked tire thermal cracking carries out CNT
Production, conversion ratio at 25-30%, provides carbon source for producing CNT continuously, and device structure is simple, low cost, instead
Answering process to be easily controlled, yield is high, has the advantages such as low, safe and environment-friendly, the non-pollutant discharge of energy consumption, has taken into account environment and money
Source problem, becomes the effective way preparing CNT.
Accompanying drawing explanation
Fig. 1 is that the present invention utilizes junked tire thermal cracking combustible gas to produce the process chart of carbon nanotube；
Fig. 2 is the structural representation of the moving bed catalyst reaction device that the present invention uses.
In figure: 1, the first speed regulator；2, the first motor；3, rotary bar；4, feeding-in solid body bucket；5, catalyst LaCoO3；6、
First thermocouple；7, the first temperature controller；8, gas access；9, the second speed regulator；10, the second motor；11, the second temperature controller；12、
Second thermocouple；13, tube furnace；14, rotating shaft；15, red copper conveyer belt；16, quartz ampoule；17, gas outlet；18, catcher.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.Following example will assist in the technology of this area
Personnel are further appreciated by the present invention, but limit the present invention the most in any form.It should be pointed out that, the ordinary skill to this area
For personnel, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement.These broadly fall into the present invention
Protection domain.
The technique of CNT prepared by a kind of combustible gas utilizing junked tire thermal cracking to produce, and comprises the following steps:
Junked tire thermal cracking: first washed by the waste tire rubber of recovery, is mingled in wherein removing some
Impurity, then send crusher in crushing, it is generally required to waste tire rubber is broken into particle diameter be 20-30 mm in size
Grain, waste tire rubber granule (containing steel wire) the feeding pyrolysis furnace after pulverizing cracks, and pyrolysis furnace is by burning combustible gas
Heating, crack under the temperature conditions of 390 DEG C-420 DEG C (such as 400 DEG C), in pyrolysis furnace, about 25-35 minute (such as
30 minutes), the air-fuel mixture gas produced from pyrolysis furnace after cracking send oil gas separation equipment to carry out Oil-gas Separation, Oil-gas Separation
Refrigerated separation tower is carried out, with cooling water, the air-fuel mixture gas entered in refrigerated separation tower is cooled down, in cooling point
Gather after condensed fuel oil carries out filter pressing from tower bottom and store, account for the combustible gas of total rubber particle weight 10% from cooling point
Enter in the moving bed catalyst reaction device of sealing above tower after effusion, after the white carbon black containing steel wire section is come out of the stove, first by cold
But auger cools down, and utilizes separation screening auger steel wire section to be separated with white carbon black simultaneously, after the steel wire section after separation is cleaned
Recycling, and white carbon black is packed after sending into flour mill pulverizing；
The generation of CNT: in the moving bed catalyst reaction device sealed, catalyst LaCoO3Pass through feeding-in solid body
Struggle against with the cloth amount of spilling of 0.25g/min by continuously and uniformly cloth be spread across moving bed quartz ampoule (Red copper transmission in 90mm*2000mm)
On band, then move into reaction zone with transmission belt with the speed of 20mm/min, with100mm*1000mm tube furnace is thermal source,
Flat-temperature zone temperature controls at 700 ± 5 DEG C, length 600mm, and the combustible gas produced during junked tire thermal cracking passes with moving bed red copper
Send the catalyst LaCoO on band3Have an effect generation CNT, due to the steering-effecting of moving bed rotating shaft, catalyst LaCoO3
After the time stopping setting on red copper conveyer belt, catalyst LaCoO3With the CNT generated on it from red copper conveyer belt
Abjection, enters catcher, and whole process is uninterrupted continuously, thus ensure that the preparation of low cost high-volume CNT.
Above-described embodiment use moving bed catalyst reaction device as in figure 2 it is shown, by first speed regulator the 1, first motor 2,
Rotary bar 3, feeding-in solid body bucket 4, catalyst LaCoO35, first thermocouple the 6, first temperature controller 7, gas access the 8, second speed governing
Device the 9, second motor the 10, second temperature controller the 11, second thermocouple 12, tube furnace 13, rotating shaft 14, red copper conveyer belt 15, quartz ampoule
16, gas outlet 17, catcher 18 form.
In the whole process technique of above-described embodiment, without any gas leak, crack under condition of negative pressure, safety
Coefficient is high, through above-mentioned technique, waste tire rubber can be converted into the about combustible gas of weight ratio 10%, the combustion of weight ratio 35%
Material oil, the white carbon black of weight ratio 35% and the steel wire of weight ratio 5%, it is achieved the recycling completely of waste tire rubber, cracking obtains
The combustible gas obtained have also been obtained sufficiently utilization, had both solved unnecessary cracking combustible gas burning and exhausting and has polluted the problem of environment, with
Time also for CNT production preparation provide carbon source.
Above the specific embodiment of the present invention is described.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformation or amendment within the scope of the claims, this not shadow
Ring the flesh and blood of the present invention.
Claims (10)
1. the technique that CNT prepared by the combustible gas utilizing junked tire thermal cracking to produce, it is characterised in that include with
Lower step: the waste tyre particle feeding pyrolysis furnace after broken is cracked, it is thus achieved that air-fuel mixture gas and solid, by described
Air-fuel mixture gas carries out Oil-gas Separation, and described solid carries out the separation of steel wire section and white carbon black；The combustion obtained after Oil-gas Separation
Oil carries out cold filtration storage, and the combustible gas obtained after Oil-gas Separation is passed through the moving bed catalyst reaction device of sealing, in catalysis
Agent LaCoO3Catalytic action under obtain CNT.
Technique the most as claimed in claim 1, it is characterised in that in described moving bed catalyst reaction device, described LaCoO3
It is spread across on the red copper conveyer belt in moving bed quartz ampoule by feeding-in solid body bucket continuously and uniformly cloth, then brings into red copper transmission
Entering reaction zone, described reaction zone is with tube furnace as thermal source, and the flat-temperature zone temperature of described tube furnace controls at 700 ± 5 DEG C, waste and old takes turns
The combustible gas that fetal heat in pregnancy cracking produces and the described LaCoO on red copper conveyer belt3Have an effect generation CNT, pass through moving bed
The steering-effecting of rotating shaft, described LaCoO3On described red copper conveyer belt after remain of a predetermined time, described LaCoO3With generation
CNT is deviate from from described red copper conveyer belt, enters catcher.
Technique the most as claimed in claim 2, it is characterised in that described LaCoO3By described feeding-in solid body bucket with 0.25g/
The cloth amount of the spilling continuous uniform cloth of min is spread across on described red copper conveyer belt.
Technique the most as claimed in claim 2, it is characterised in that described red copper conveyer belt moves into the speed of 20mm/min
Enter described reaction zone.
Technique the most as claimed in claim 2, it is characterised in that the external diameter of described moving bed quartz ampoule is 90mm, a length of
2000mm, the external diameter of described tube furnace is 100mm, a length of 1000mm, a length of 600mm of the flat-temperature zone of described tube furnace.
Technique the most as claimed in claim 1, it is characterised in that the temperature of described cracking is 390 DEG C～420 DEG C, the time is
25～35 minutes.
Technique the most as claimed in claim 6, it is characterised in that the temperature of described cracking is 400 DEG C, the time is 30 minutes.
Technique the most as claimed in claim 1, it is characterised in that before carrying out described cracking, junked tire is first carried out
Pretreatment, the process of described pretreatment is as follows: carry out washing with removal of contamination, then by junked tire by the junked tire of recovery
Send the granule that crusher in crushing becomes particle diameter to be 20～30 mm in sizes.
Technique the most as claimed in claim 1, it is characterised in that described air-fuel mixture gas carries out the process of Oil-gas Separation such as
Under: air-fuel mixture gas is sent into refrigerated separation tower and is carried out Oil-gas Separation, mixes with the cooling water oil gas to entering in refrigerated separation tower
Closing gas to cool down, combustible gas escapes above refrigerated separation tower, gathers condensation in the bottom of refrigerated separation tower and forms fuel
Oil, stores after fuel oil carries out filter pressing.
Technique the most as claimed in claim 1, it is characterised in that described solid carries out separating steel wire section and the process of white carbon black
As follows: after described solid is come out of the stove, first cooled down by cooling auger, and utilize separation screening auger by steel wire section and charcoal simultaneously
Black separation, the steel wire section after separation recycles after cleaning, and white carbon black is packed after sending into flour mill pulverizing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610527586.6A CN106185863A (en) | 2016-07-06 | 2016-07-06 | The technique that CNT prepared by the combustible gas utilizing junked tire thermal cracking to produce |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610527586.6A CN106185863A (en) | 2016-07-06 | 2016-07-06 | The technique that CNT prepared by the combustible gas utilizing junked tire thermal cracking to produce |
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| CN106185863A true CN106185863A (en) | 2016-12-07 |
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| CN201610527586.6A Pending CN106185863A (en) | 2016-07-06 | 2016-07-06 | The technique that CNT prepared by the combustible gas utilizing junked tire thermal cracking to produce |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107381541A (en) * | 2017-08-03 | 2017-11-24 | 中创奕龙科技股份有限公司 | A kind of preparation method for carbon nano-tube using cracking black carbon as carbon source |
| CN112744804A (en) * | 2019-10-29 | 2021-05-04 | 中国石油化工股份有限公司 | Method for preparing carbon material from heavy oil slurry |
| CN115010110A (en) * | 2022-07-06 | 2022-09-06 | 西安交通大学 | Method for preparing hard carbon-graphene composite material by comprehensively utilizing waste tire pyrolysis product |
Citations (3)
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|---|---|---|---|---|
| CN1317446A (en) * | 2000-04-13 | 2001-10-17 | 中国科学院成都有机化学研究所 | Moving-bed catalytic cracking process for continuously preparing nm carbon tubes |
| CN101935540A (en) * | 2009-06-30 | 2011-01-05 | 上海绿人生态经济环境保护研究所 | Innocuous treatment technology for waste rubber by adding catalyst comprising steel wire |
| CN105349161A (en) * | 2015-11-06 | 2016-02-24 | 河北工业大学 | Method for producing hydrogen and carbon nanotubes through pyrolysis of waste tyres and biomass |
-
2016
- 2016-07-06 CN CN201610527586.6A patent/CN106185863A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317446A (en) * | 2000-04-13 | 2001-10-17 | 中国科学院成都有机化学研究所 | Moving-bed catalytic cracking process for continuously preparing nm carbon tubes |
| CN101935540A (en) * | 2009-06-30 | 2011-01-05 | 上海绿人生态经济环境保护研究所 | Innocuous treatment technology for waste rubber by adding catalyst comprising steel wire |
| CN105349161A (en) * | 2015-11-06 | 2016-02-24 | 河北工业大学 | Method for producing hydrogen and carbon nanotubes through pyrolysis of waste tyres and biomass |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107381541A (en) * | 2017-08-03 | 2017-11-24 | 中创奕龙科技股份有限公司 | A kind of preparation method for carbon nano-tube using cracking black carbon as carbon source |
| CN112744804A (en) * | 2019-10-29 | 2021-05-04 | 中国石油化工股份有限公司 | Method for preparing carbon material from heavy oil slurry |
| CN115010110A (en) * | 2022-07-06 | 2022-09-06 | 西安交通大学 | Method for preparing hard carbon-graphene composite material by comprehensively utilizing waste tire pyrolysis product |
| CN115010110B (en) * | 2022-07-06 | 2024-03-22 | 西安交通大学 | Method for preparing hard carbon-graphene composite material by comprehensively utilizing pyrolysis products of waste tires |
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