CN100434359C - Method and device for continuously producing nanometer carbon material - Google Patents
Method and device for continuously producing nanometer carbon material Download PDFInfo
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- CN100434359C CN100434359C CNB2005100036112A CN200510003611A CN100434359C CN 100434359 C CN100434359 C CN 100434359C CN B2005100036112 A CNB2005100036112 A CN B2005100036112A CN 200510003611 A CN200510003611 A CN 200510003611A CN 100434359 C CN100434359 C CN 100434359C
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Abstract
The present invention relates to a method for continuously producing a nanometer carbon material. A gas reactant and a catalyst contact. Reaction temperature is from 100 to 1200 DEG C, and reaction pressure is from 0.01 to 10MPa. The airspeed of the gas reactant is from 500 to 50000 ml/g of catalyst/hour, the ratio of the conveying speed of the catalyst to the cross sectional area of a reaction tube is from 0.02 to 10 g/h/cm<2>. A device of the present invention is as follows: one end of a tubular reactor is provided with a feeding zone, and a catalyst feeding opening and a gas reactant gas inlet are arranged in the feeding zone. The middle section in the tubular reactor is provided with a heatable reaction zone. The other end of the tubular reactor, which corresponds to a feeding end, is provided with a gas and solid separation zone. The gas and solid separation zone is provided with an end gas outlet and a discharging opening. A cooling zone is arranged between the heatable reaction zone and the gas and solid separation zone. A straight tube is matched at the center of the tubular reactor in an axial direction. One end of the straight tube, which is positioned in the tubular reactor, is closed, and the other end of the straight tube is opened to be inserted into a thermocouple. A lifting device is matched with the feeding end of the tubular reactor.
Description
Technical field
The present invention relates to a kind of method of under the catalyzer existence condition, producing nano-carbon material.
The invention still further relates to a kind of device that is used to realize aforesaid method.
Technical background
Nano-carbon material has unique physical and chemical performance, can be used for producing various matrix materials such as electrical shielding material etc.In the production process of nano-carbon material such as carbon nanotube and carbon nano fiber, carbon raw material gas such as various hydro carbons contact with catalyzer at a certain temperature, and scission reaction will take place hydro carbons, generate the solid nano carbon material, generate other gaseous product such as hydrogen simultaneously.Because this process has solid product to generate, if so adopt at the widely used fixed-bed reactor of catalytic field then must adopt periodical operation (as described in Chinese patent CN 1166826C), nano-carbon material can not take out from reactor continuously, therefore after carrying out certain hour, reaction must get off thalidomide, take out nano-carbon material, add catalyzer again and heat up again and react, this periodical operation causes process efficiency low, and product is also unstable.
A kind of improvement to said fixing bed catalytic process is the catalysis method that flows.Among the relative merits Chinese patent CN 1061706C of mobile catalysis method detailed commentary is arranged.Chinese patent CN 1378974A also discloses a kind of method and device of continuous production CNT (carbon nano-tube), adopts the air operated mode that catalyzer is blown into reactor, and the CNT (carbon nano-tube) that generates is blown out reactor.The turndown ratio of this mode feed gas flow rates is very little, and gas flow rate is little then can not to play effective conveying effect, gas flow rate greatly then in reactor the residence time short, the unstripped gas transformation efficiency is low, CNT (carbon nano-tube) length can shorten, and collects also more difficult.And according to the equipment structure chart that patent specification provides, the tail gas outlet pipe, separates not in same gas circuit with the product collector, is difficult to that product is carried out continuous effective ground and collects.
Chinese patent CN 1061706C discloses a kind of preparation method of gas-phase grown nanometer carbon fibre, by being changed at 0-60 ℃, reaction zone and sea line angle adjust the residence time of catalyzer in reactor, but owing to can't overcome the stop plugging problem of carbon nano fiber in reaction tubes, the long-time continuous that still can't realize loading greatly running.
As seen, the production technique of nano-carbon material also requires further improvement.
Summary of the invention
The object of the present invention is to provide a kind of method of continuous production nano-carbon material.
Another purpose of the present invention is to provide a kind of device that is used to realize aforesaid method.
For achieving the above object, the method of continuous production nano-carbon material provided by the invention is with in gas reactant and the continuous input reactor of catalyzer, gas reactant is stirred with catalyzer contact, under certain temperature and pressure, the continuous production nano-carbon material.
The gases used reactant of the present invention is Sweet natural gas, liquefied gas, methane, ethane, propane, butane, acetylene, carbon monoxide, carbonic acid gas or contains one or more gas mixture in above-mentioned, wherein preferred Sweet natural gas or liquefied gas.
The preferred carbon nano fiber of product nano-carbon material, carbon nanotube, nano-carbon powder that the present invention prepares, wherein preferred carbon nano fiber, carbon nanotube.Preferred carbon nano fiber or carbon nanotube diameter are the 3-500 nanometer, more preferably the 5-100 nanometer.The length of carbon nano fiber or carbon nanotube is not limit, and preferred carbon nano fiber or length of carbon nanotube are the 10-10000 micron.
The used catalyzer of the present invention can be known to producing the effective any catalyzer of nano-carbon material.For example load or unsupported VIII family metal are the catalyzer of known production nano-carbon material.Preferred iron, cobalt and nickel, more preferably cobalt and nickel, most preferably nickel in these metals.In the catalyzer of load, carrier is the inorganic high-temperature resistant oxide compound, wherein preferred aluminum oxide, silicon-dioxide, silica-alumina, carbon nanotube or carbon nano fiber, more preferably carbon nanotube or carbon nano fiber, be carrier most preferably, so that the recovery of catalyst component and avoid the introducing of other impurity with the product nano-carbon material.Preferred unsupported catalyzer in load and unsupported catalyzer is so that the recovery of catalyst activity component.Catalytically-active metals exists with the weight percentage of 1-100wt% usually, preferred 10-99wt%.Also can add promotor in the catalyzer, and be that catalysis method production nano-carbon material field is known.Auxiliary agent comprises lanthanum, cerium, yttrium, zirconium, copper or contains the compound of above-mentioned element, and exists with the amount that is less than the main catalytic metal usually, and promotor is 1: 99 to 40: 60 with the element wt ratio of main catalytic metal.Preferred promoter is yttrium and zirconium.Catalyzer is sphere or irregular particle or Powdered, the preferred powder powder.The granularity of catalyzer is the 1-3000 micron, preferred 20-150 micron.
Temperature of reaction of the present invention is 100-1200 ℃, and preferred temperature of reaction is 400-900 ℃.
Reaction pressure of the present invention is 0.01-10Mpa, and preferred pressure is 0.05-1Mpa, and most preferred pressure is 0.1-0.2Mpa.
Gas reactant air speed of the present invention be the 500-50000ml/g catalyzer/hour, catalyst transport speed is 0.02-10g/h/cm with the ratio of reaction tubes cross-sectional area
2
The device that is used to realize aforesaid method provided by the invention, its primary structure is:
One tubular reactor, one end are feed end, and this feed end is provided with a catalyst feeds and gas reactant inlet mouth.
The stage casing of this reactor is a reaction zone, is provided with well heater at reaction zone, makes reaction zone can reach the required temperature of reaction.
The corresponding the other end of this reactor and feed end is the gas solid separation district, and this gas solid separation district is provided with tail gas outlet and drain hole, and wherein the tail gas outlet is towards the top, and drain hole is towards the below.
Between reaction zone and gas solid separation district a cooling zone is arranged, the cooling zone is furnished with radiator element and/or water-cooled chuck.
The tubular reactor central shaft is to being furnished with a straight tube, and this straight tube is positioned at the end sealing of reactor, and the other end opening is used to insert the temperature in the thermocouple measurement reactor.
The feed end of above-mentioned tubular reactor is furnished with lifting device, makes reactor adjustable between 0-30 ° of horizontal tilt angle, and preferred horizontal tilt angle is 1-20 °.
This tubular reactor is connected with motor and linkage system and speed regulation device, and the rotating speed that makes reactor is adjustable between the 60-1200 commentaries on classics/h, and the rotating speed of preferred reactor is 120-600 commentaries on classics/h.
The straight tube of above-mentioned reactor center can be an immobilized, also can be furnished with motor and linkage system, and straight tube can be rotated.The straight tube rotating speed of preferred above-mentioned reactor center is adjustable between the 60-1200 commentaries on classics/h, and preferred rotating speed is 120-600 commentaries on classics/h.
The reaction tube of reactor can be furnished with one or more baffle plate, and preferred baffle plate number is the 2-8 piece, most preferably 4.The direction of baffle plate is parallel with reaction tubes, also can be angled, and wherein the direction of preferred baffle plate is parallel with reaction tubes.The effect of baffle plate is that the catalyst fines that will manage the bottom in the reaction tubes rotation process brings to reaction tubes top on the one hand, make catalyst fines then because action of gravity is landed, and has promoted fully contacting of catalyzer and reactant gas; Can prevent the nano-carbon material wall built-up of catalyzer or generation on the other hand, block reaction tubes; In addition, because reaction tubes tilts at a certain angle, the nano-carbon material that catalyzer and reaction zone generate is got on by baffle belt repeatedly in reaction tubes and falls, and makes that solid materials constantly moves to Way out in the reaction tubes, has realized the automatic transport of solids stream in reactor.Reaction tube diameter, angle of inclination and rotating speed have determined the residence time of material in reaction tubes, and can therefore realize the adjusting to the nano-carbon material growth time, can therefore change size such as the diameter and the length of nano-carbon material.The size of nano-carbon material such as diameter and length are also relevant with reactant gas flow rate and temperature of reaction, reaction pressure, selected catalyzer, and the appeal factor all can be regulated easily with method of the present invention.Wherein according to selected catalyzer, reactant, temperature of reaction and pressure, the nano-carbon material of generation can be carbon nano fiber, carbon nanotube, nano-carbon powder, preferred Nano carbon fibers peacekeeping carbon nanotube, most preferably carbon nano fiber.
The straight tube outer wall of reactor center can be furnished with and tubular reactor axially parallel or one or more angled fin.The effect of fin is further to prevent the nano-carbon material wall built-up that generates, blocks reaction tubes.
Cooling zone between reaction zone and the gas solid separation district, its effect is that the gas, the solid mixture stream that make the gaseous product that contains nano-carbon material, catalyzer, unreacted unstripped gas and reaction generation were introduced into the cooling zone and are cooled before entering the gas solid separation district, reaction owing to reducing, temperature is stopped, prevent that the gas solid separation district is at high temperature blocked because the continuation of reaction takes place, also make simultaneously operational safety, and reduce the material requirement of the device after the cooling zone.
Above-mentioned gas, solid mixture stream come out to enter the gas solid separation district from the cooling zone.The gas solid separation district has inlet, is used for gas, solid mixture stream after above-mentioned being cooled; The tail gas outlet, the gas stream after being used to separate; Drain hole, the solids stream after being used to separate.The gas solid separation district can be furnished with box settling vessel or cyclonic separator, preferred box settling vessel.
Because tubular reactor itself rotates, so the connection between catalyzer charging zone and tubular reactor, and being connected between tubular reactor and the gas solid separation district select dynamic seal for use.Can use any known valid dynamic seal mode.
The present invention can operate with intermittence or successive mode, the preferred latter.
The solids stream that the present invention will contain catalyzer is imported reaction zone continuously by the catalyzer charging zone.The solids stream that wherein contains catalyzer can be selected any known valid mode of movement in the conveying of catalyzer charging zone, has used the screw feeder in the preferred embodiments of the invention, and the screw feeder can be by driven by motor.
The present invention uses said apparatus to realize the method for continuous production nano-carbon material, and its flow process is:
A) solids stream that will contain catalyzer is imported reaction zone continuously by the catalyzer charging zone;
B) gas stream that will contain gas reactant feeds reaction zone continuously;
C) reaction zone is positioned at the rotatable tubular reactor of tiltable, and is heated to certain temperature;
D) catalyzer and gas reactant contact under certain temperature and pressure and react at reaction zone, and partly or entirely gas reactant generation chemical conversion generates nano-carbon material and other gaseous product such as hydrogen;
E) contain the gas, solid mixture stream of the gaseous product that nano-carbon material, catalyzer, unreacted gas reactant and reaction generate along with the rotation of reactor is moved out of reaction zone;
F) above-mentioned gas, the solid mixture stream that contains the gaseous product of nano-carbon material, catalyzer, unreacted gas reactant and reaction generation is admitted to the gas solid separation district after reaction zone output;
G) gas stream that obtains of gas solid separation district is discharged by the tail gas outlet in gas solid separation district;
H) solids stream that contains nano-carbon material that the gas solid separation district obtains is exported and is collected by the drain hole in gas solid separation district.
Compare with the production method of conventional nano-carbon material, the advantage of the inventive method is the employing by the rotatable tubular reactor of tiltable, realized the serialization production of nano-carbon material fully, reactor can turn round under high loading, there is not the blockage problem of reaction tubes in long-time running, and not only process operation efficient improves greatly, and the operation operating mode is easy to adjust, and the interference that does not stop, goes into operation, constant product quality.
Description of drawings
Fig. 1 is the synoptic diagram of a kind of embodiment of the present invention.
Fig. 2 is the synoptic diagram of tubular reactor and central straight pipe structure.
Embodiment
In conjunction with Fig. 1.The solids stream that contains catalyzer in the catalyst hooper (2) is imported reaction zone (6) continuously by catalyzer charging zone (1); The gas stream that will contain gas reactant feeds reaction zone (6) continuously by gas feed mouth (3); Reaction zone (6) is positioned at the rotatable tubular reactor of tiltable (4), and is heated stove (5) and is heated to certain temperature; Catalyzer and gas reactant contact under certain temperature and pressure and react at reaction zone (6), and partly or entirely gas reactant generation chemical conversion generates nano-carbon material and other gaseous product such as hydrogen; The gas, solid mixture stream that contain the gaseous product that nano-carbon material, catalyzer, unreacted gas reactant and reaction generate are along with the rotation of reactor (4) is moved out of reaction zone (6); The above-mentioned gas that contains the gaseous product that nano-carbon material, catalyzer, unreacted unstripped gas and reaction generate, solid mixture stream are admitted to cooling zone (8) after the reaction zone output and are cooled; Cooled above-mentioned gas, solid mixture flow to into the gas solid separation district (10); The gas stream that gas solid separation district (10) obtains is discharged by the tail gas outlet (9) in gas solid separation district; The solids stream that contains nano-carbon material that gas solid separation district (10) obtains is exported and is collected by the drain hole (12) in gas solid separation district.(7) are the straight tube at reactor (4) center among Fig. 1.(11) be thermopair in the straight tube, be used for measuring reaction zone temperature.
Fig. 2 is the possibility of tubular reactor and central straight pipe structure.(a) for tubular reactor is unworthy of baffle plate, central straight pipe is not with fin, tubular reactor rotation and central straight pipe is static; (b) join baffle plate for tubular reactor, central straight pipe is not with fin, tubular reactor rotation and central straight pipe is static; (c) join baffle plate for tubular reactor, central straight pipe racks fin, tubular reactor rotate simultaneously with central straight pipe and direction opposite; (d) for tubular reactor is unworthy of baffle plate, central straight pipe racks fin, tubular reactor rotate simultaneously with central straight pipe and direction opposite.The preferred embodiments of the invention are (c).
Embodiment 1:
Adopt diameter 96mm, the rotatable tubular reactor of long 1400mm adopts above-mentioned continuous processing operation provided by the present invention, with the liquefied gas is raw material, air speed be the 500ml/g catalyzer/hour, catalyzer is NiZr, catalyst transport speed is 10g/h/cm with the ratio of reaction tubes cross-sectional area
2, reaction pressure 0.1MPa, 100 ℃ of temperature of reaction, the carbon nano fiber formation speed is 1200g/h.
Embodiment 2:
Liquefied gas is a raw material, air speed be the 50000ml/g catalyzer/hour, catalyst transport speed is 0.02g/h/cm with the ratio of reaction tubes cross-sectional area
2, reaction pressure 10MPa, 1200 ℃ of temperature of reaction, all the other are with embodiment 1, and the carbon nano fiber formation speed is 1300g/h.
Comparative example:
Adopt diameter 96mm, the fixed-bed reactor of long 1400mm, adopt periodical operation, with the liquefied gas is raw material, air speed be the 15000ml/g catalyzer/hour, catalyzer is NiZr, catalyzer loading amount 5g, 3 hours afterreaction pipes of 650 ℃ of reactions of normal pressure seriously stop up, and this moment, the carbon nano fiber growing amount was 150g, average 50g/h; Adopt the rotatable tubular reactor of same size, adopt continuous processing operation provided by the present invention, raw material, catalyzer, air speed, temperature, pressure are identical with said process, catalyst transport speed is 40g/h, 3 hours no latch up phenomenons of operate continuously, the carbon nano fiber formation speed is 1200g/h, and production efficiency is 24 times of fixed bed periodical operation.
Claims (12)
1. the method for a continuous production nano-carbon material, gas reactant is contacted with catalyzer, temperature of reaction 100-1200 ℃, reaction pressure 0.01-10Mpa, the gas reactant air speed be the 500-50000ml/g catalyzer/hour, catalyst transport speed is 0.02-10g/h/cm with the ratio of reaction tubes cross-sectional area
2, reacted gas, solid mixture stream refrigerated separation obtain nano-carbon material;
Reaction zone is positioned at the rotatable tubular reactor of tiltable, and the horizontal tilt angle of this tubular reactor is 1-20.；
Described gas reactant is Sweet natural gas, methane, ethane, propane, butane, acetylene, carbon monoxide, carbonic acid gas or contains one or more gas mixture in above-mentioned;
Described catalyzer is the catalyzer of unsupported VIII family metal, and 1-100% exists with weight percentage; Catalyzer is sphere or irregular particle shape, and its granularity is the 1-3000 micron.
2. the method for claim 1 is characterized in that, catalyzer is the catalyzer of the VIII family metal of load, and carrier is aluminum oxide, silicon-dioxide, silicon-dioxide one aluminum oxide, carbon nanotube or carbon nano fiber.
3. the method for claim 1 is characterized in that, also adds promotor in the catalyzer, and promotor comprises lanthanum, cerium, yttrium, zirconium, copper or contain the compound of above-mentioned element that promotor is 1: 99 to 40: 60 with the element wt ratio of main catalytic metal.
4. the method for claim 1 is characterized in that, the nano-carbon material for preparing is carbon nano fiber, carbon nanotube or nano-carbon powder; Carbon nano fiber or carbon nanotube diameter are the 3-500 nanometer, and length is the 10-10000 micron.
5. claim 1 or 2 method is characterized in that VIII family metal is iron, cobalt or nickel.
6. device that is used to realize the described method of claim 1, main composition is:
One tubular reactor, one end are intake zone, and this intake zone is provided with a catalyst feeds and gas reactant inlet mouth;
Stage casing in this tubular reactor is a reaction zone, is provided with well heater at reaction zone, to provide reaction required temperature;
The corresponding the other end of this tubular reactor and feed end is the gas solid separation district, and this gas solid separation district is provided with tail gas outlet and drain hole, and wherein the tail gas outlet is towards the top, and drain hole is towards the below;
Between reaction zone and gas solid separation district a cooling zone is arranged, the cooling zone is furnished with radiator element and/or water-cooled chuck;
This tubular reactor central shaft is to being furnished with a straight tube, and this straight tube is positioned at the end sealing of tubular reactor, and the other end opening is used to insert the temperature in the thermocouple measurement reactor;
The feed end of above-mentioned tubular reactor is furnished with lifting device, makes tubular reactor adjustable between 1-20 ° of horizontal tilt angle;
Above-mentioned tubular reactor is connected with motor and linkage system and speed regulation device, and it is adjustable between the 60-1200 commentaries on classics/h making the tubular reactor rotating speed;
By said apparatus:
A) solids stream that will contain catalyzer is imported reaction zone continuously;
B) gas stream that will contain gas reactant feeds reaction zone continuously;
C) reaction zone is positioned at rotatable tubular reactor, and is heated to certain temperature;
D) catalyzer and gas reactant contact and react at reaction zone, and partly or entirely gas reactant generation chemical conversion generates nano-carbon material and other gaseous product;
E) contain the gas, solid mixture stream of the gaseous product that nano-carbon material, catalyzer, unreacted gas reactant and reaction generate along with the rotation of reactor is moved out of reaction zone;
F) above-mentioned gas, the solid mixture stream that contains the gaseous product of nano-carbon material, catalyzer, unreacted unstripped gas and reaction generation is admitted to the gas solid separation district after reaction zone output;
G) gas stream that obtains of gas solid separation district is discharged by the tail gas outlet in gas solid separation district;
H) solids stream that contains nano-carbon material that the gas solid separation district obtains is exported and is collected by the drain hole in gas solid separation district.
7. the device of claim 6 is characterized in that, the tubular reactor central straight pipe is furnished with motor and linkage system, and straight tube can be rotated, and rotating speed is adjustable between the 60-1200 commentaries on classics/h.
8. the device of claim 6 is characterized in that, the reaction tube of tubular reactor is furnished with at least one baffle plate, and the direction of baffle plate is parallel with reaction tubes, or at angle.
9. the device of claim 6 is characterized in that, the straight tube outer wall at tubular reactor center is furnished with and tubular reactor axially parallel or angled at least one fin.
10. the device of claim 6 is characterized in that, the gas solid separation district is furnished with box settling vessel or cyclonic separator.
11. the device of claim 6 is characterized in that, being connected between tubular reactor and the intake zone, and tubular reactor is connected with the dynamic seal that is connected between the gas solid separation district.
12. the device of claim 6 is characterized in that, the screw feeder is adopted in the conveying of catalyst solid material in the intake zone.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100036112A CN100434359C (en) | 2005-01-05 | 2005-01-05 | Method and device for continuously producing nanometer carbon material |
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| CNB2005100036112A CN100434359C (en) | 2005-01-05 | 2005-01-05 | Method and device for continuously producing nanometer carbon material |
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| CN1800006A CN1800006A (en) | 2006-07-12 |
| CN100434359C true CN100434359C (en) | 2008-11-19 |
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| CNB2005100036112A Expired - Fee Related CN100434359C (en) | 2005-01-05 | 2005-01-05 | Method and device for continuously producing nanometer carbon material |
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Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100956352B1 (en) * | 2007-09-06 | 2010-05-07 | 세메스 주식회사 | Apparatus and method of producting carbon nano tube |
| KR101239168B1 (en) * | 2008-08-08 | 2013-03-05 | 가부시끼가이샤 도시바 | Nanocarbon generation device |
| CN105000543A (en) * | 2014-04-18 | 2015-10-28 | 中国科学院成都有机化学有限公司 | Method for preparing aligned carbon nanotubes |
| CN105271164B (en) | 2014-07-17 | 2019-08-20 | 山东大展纳米材料有限公司 | A kind of device and method of continuously preparing nm carbon tubes |
| CN107311146A (en) * | 2016-04-25 | 2017-11-03 | 山西中兴环能科技有限公司 | A kind of serialization prepares the device and method of nano-carbon material |
| CN107337193A (en) * | 2016-04-29 | 2017-11-10 | 山西中兴环能科技有限公司 | A kind of reactor rotation prepares the device and method of nano-carbon material |
| CN107413138A (en) * | 2016-05-18 | 2017-12-01 | 山西中兴环能科技有限公司 | A kind of exhaust treatment system and the continuous device for preparing nano-carbon material |
| KR102047370B1 (en) * | 2016-07-14 | 2019-11-22 | 주식회사 엘지화학 | Apparatus for drying and collecting carbon nanotube product and process for preparing carbon nanotubes |
| CN108311064A (en) * | 2017-01-16 | 2018-07-24 | 赵社涛 | A kind of Horizontal stirring reactor for carbon nanotube production |
| CN109261100B (en) * | 2018-08-21 | 2020-08-25 | 浙江工业大学 | Reaction system for preparing carbon material |
| IT201800021040A1 (en) * | 2018-12-24 | 2020-06-24 | Danilo Vuono | Solid support, system, and processes |
| CN110451486B (en) * | 2019-08-08 | 2022-11-22 | 江西铜业技术研究院有限公司 | Device and method for preparing carbon nanotubes in batches |
| CN111115614B (en) * | 2019-10-12 | 2020-09-25 | 成都科汇机电技术有限公司 | Carbon nano tube prepared by catalytic cracking of hydrocarbon by rotary method, device and method |
| CN111072008A (en) * | 2019-12-24 | 2020-04-28 | 陕西延长石油(集团)有限责任公司研究院 | Equipment and method for continuously preparing carbon material through gas-solid reaction |
| CN112705150B (en) * | 2020-11-05 | 2022-12-23 | 中国恩菲工程技术有限公司 | Composite material preparation device and method |
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