CN109809374A - A kind of push boat type semi-continuous process boron nitride nano-tube prepares furnace and its application method - Google Patents
A kind of push boat type semi-continuous process boron nitride nano-tube prepares furnace and its application method Download PDFInfo
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Abstract
The present invention relates to a kind of push boat type semi-continuous process boron nitride nano-tubes to prepare furnace and its application method.The set equipment includes electric control temperature heating device A, furnace body B, burner C and furnace tail D, electric control temperature heating device A is used to adjust the temperature of control furnace body B, burner hearth in furnace body B is connected by boiler tube with the burner C of two sides and furnace tail D, is provided in outer surface of furnace tube for cooling recirculated water support.Raw material is reacted in furnace body B burner hearth with ammonia, is then transferred in the boiler tube between furnace body B and furnace tail D and is cooled down, while next group raw material is transported in burner hearth and is reacted, and the product cooled down takes out from furnace tail D, it is thus achieved that continuous production.The device has many advantages, such as that easy to operate, product structure is rich and varied, is particularly suitable for industrialized production and application, and device security is high, stability is good, can continuously synthesize the BNNTs of different structure on a large scale.
Description
Technical field
The present invention relates to mechanical and inorganic non-metallic material synthesis technical fields, and in particular to a kind of push boat type semi-continuous process
Boron nitride nano-tube prepares furnace and its application method.
Background technique
The synthetic method of boron nitride (BN) occupies extremely important status in the research of boron nitride material.Develop one kind
The method of the extensive synthesis higher degree boron nitride of industrialization can provide solid for the theoretical research of boron nitride and practical application
Basis and guarantee.
Boron nitride nano-tube (BNNTs) is one kind more important in numerous boron nitride materials, with excellent machinery,
The performances such as calorifics, electromagnetism.Existing BNNTs preparation method mainly includes arc discharge method, laser ablation method, vapour deposition process
(CVD), high-temperature synthesis etc..Wherein arc discharge method directly uses reaction raw materials as electrode, is then obtained by arc discharge
Target material, BNNTs are exactly to be prepared for the first time using this method.But energy consumption is high for this method, is not suitable for batch production.Swash
Light ablation is bombarded blocky reactant in high-pressure inert gas atmosphere using laser and obtains required product, and this method disadvantage is energy
Consumption height, low output, are not suitable for commercial introduction and industrialization.Chemical vapour deposition technique (CVD) basic principle: sharp in reactive atmosphere
It is chemically reacted after being in contact with gas reactant with solid reactant, finally obtains stable solid product.This method is wanted
Want to succeed, there is following three points necessary condition: (1) under depositing temperature, reactant has enough vapour pressures, and can be with suitable
When speed be introduced into reaction chamber;(2) reactant is other than forming solid film substance, it is necessary to be volatile;(3) it deposits
Film and basis material must have sufficiently low vapour pressure.It follows that CVD method the high requirements on the equipment, has very big
Limitation, usually more preparations for being used for coating material.
High-temperature synthesis is a kind of most common method, and proportioned raw material be sufficiently mixed making it by this method first
It is uniformly dispersed, then carries out physical-chemical reaction under high temperature environment, generate crude product, finally by the techniques such as removal of impurities, dry
Obtain target product.This method have many advantages, such as it is easy to operate, it is relatively low to equipment requirement.Performance is stable, safe and reliable
High―temperature nuclei equipment is the basic guarantee that raw material sufficiently reacts at high temperature.Chinese patent CN201359434Y discloses one kind and pushes away
Two pipe reduction furnace of boat formula, and it is used for the reduction of metal powder, but on the one hand the apparatus structure is complex, temperature control area
It is more, temperature difference is small, the synthesis of BNNTs is not made much sense;On the other hand the device does not have gas-circulating system, for
The effective rate of utilization of reducing gas is not high.Chinese patent CN104555990A discloses a kind of carbonized graphite continuous type high temperature furnace
And its application method, and it is used for the synthesis of graphite material respectively.However the equipment does not simply fail to build atmosphere needed for reacting,
And the exhaust gas that reaction generates cannot also be effectively treated, and there are environmental issues;Furthermore there are different thermotonuses for the equipment
Area causes heating equipment more, and material need to promote in differential responses section, inconvenient.
Summary of the invention
The present invention provides a kind of semicontinuous boron nitride nano-tube of push boat type and prepares furnace, which belongs to semicontinuous preparation
Device reduces the equipment unnecessary cooling time by high temperature to low temperature, considerably reduces energy consumption, improve using the longevity
Life is particularly suitable for a variety of different types of presomas and (reaches as high as 1600 DEG C) at different temperatures quickly, largely synthesizes
BNNTs.To achieve the above object, the technical solution adopted in the present invention is specific as follows:
A kind of semicontinuous boron nitride nano-tube of push boat type prepares furnace, including electric control heating arrangement A, furnace body B, burner C, furnace tail
D and push rod.Electric control heating arrangement A is fixed on furnace body B, for carrying out heat temperature raising under controlled conditions for furnace body B;In furnace
It is provided with burner exhaust pipe 1 on head C, furnace tail air inlet pipe 2 is provided on furnace tail D;Burner C and furnace tail D passes through boiler tube 14 and furnace
Burner hearth 8 in body B is connected, and forms complete gas access way.Push rod can enter burner B's by burner C and boiler tube 14
In burner hearth 8, and the product in burner hearth 8 is pushed into the boiler tube between furnace tail D and furnace body B.On the one hand this measure is next batch materials
It reacts and vacates position, reaction products therefrom is on the other hand transferred to cooling zone and is cooled down to come out of the stove.
Further, electric control heating arrangement A includes power control cabinet and heating element (1800 type high temperature Si-Mo rod), power control cabinet energy
Enough control heating element carries out heat temperature raising to furnace body B according to the program of setting, so that the temperature in burner hearth is stablized in setting value.
Electric control heating arrangement A use PID intelligent program temperature control, Temperature Control, electrical equipment control integrated synthesis control function,
Main control circuit is the temperature control loop being made of bidirectional triode thyristor, auto-transformer, relay and intelligent temperature controller.
Intelligent temperature controller is using number display, and 0.3 grade of measurement accuracy, 30 sections of temperature programmed controls, control by reachable ± 1 DEG C of temperature-controlled precision
Mode used phase shift to touch method, and instrument can be adjusted manually or automatically.
Furnace body B includes furnace shell 7, burner hearth 8, furnace lining 9, insulating layer 10.It is arranged in around the burner hearth 8 inside furnace body B and is enclosed with
Furnace lining 9 is enclosed with insulating layer 10 and furnace shell 7 outside furnace lining 9.The furnace shell 7 uses 304 stainless steel plate machine-shapings, possesses
Enough intensity and rigidity and good appearance, furnace shell is totally using the double-deck air-cooled structure.Burner hearth 8 is produced using Shanghai Aesop Lai Te
1700 type crystal fibre machine-shapings;Furnace lining 9 is that 1600 type alumina hollow balls fill the compound Lining to be formed, and has insulation
Performance is good, anti-rapid heating and cooling, without consider thermal stress influence, energy conservation, high, indeformable intensity the advantages that;Insulating layer 10 is 1500
The high-quality mullite light thermal-insulation brick masonry of type.Furnace bottom supports boiler tube using high temperature mullite insulating brick, prevents boiler tube heat distortion.
Burner C includes burner exhaust pipe 1, burner fire door 3, stove head seal cover 5, burner table 11, burner recirculated water support 15-1.
Burner exhaust pipe 1 is connected with boiler tube 14, for vacuumizing and being discharged the exhaust gas in burner hearth;Burner recirculated water support 15-1 is socketed in
Behind 14 outer surface of boiler tube, one end is fixed on the other end on burner table 11 and is fixed on furnace body B by flange 16.Burner recirculated water support
On the one hand can play the role of the equipment such as fixed, support boiler tube prevents it from moving, on the other hand can also be by cooling water to furnace
Pipe etc. cools down.Burner table 11, burner recirculated water support 15-1 etc. are wrapped in interior and carried out to it close by stove head seal cover 5
Envelope, is provided with burner exhaust pipe 1 on stove head seal cover 5, and burner fire door 3 is arranged in 14 one end of boiler tube.
Furnace tail D is similar with burner C-structure, including furnace tail air inlet pipe 2, furnace tail seal closure 6, furnace tail fire door 4, furnace tail table 12,
Furnace tail recirculated water support 15-2.Furnace tail air inlet pipe 2 is connected with boiler tube 14, for conveying unstripped gas ammonia into burner hearth;Furnace tail follows
Ring water support 15-2 is socketed in 14 outer surface of boiler tube and forms cooling zone, and the one end furnace tail recirculated water support 15-2 is fixed on furnace tail table 12 separately
One end is fixed on furnace body B by flange 16.The effect of furnace tail recirculated water support is similar with the effect of burner recirculated water support.Furnace tail is close
Furnace tail table 12, furnace tail recirculated water support 15-2 etc. are wrapped in interior and are sealed to it by sealing cover 6, are arranged on furnace tail seal closure 6
There is furnace tail air inlet pipe 2, furnace tail fire door 4 is arranged in 14 other end of boiler tube.
Further, furnace tail recirculated water support 15-1 and the outer surface burner recirculated water support 15-2 be provided with stainless steel tube 13,
Stainless steel protection cover is provided with adjustment base 18 in burner table 11 and 12 bottom of furnace tail table, and furnace tail recirculated water support 15-1, burner follow
Ring water support 15-2 is connected with cooling water.
Further, gas-recycling plant, such as pipeline are additionally provided between burner exhaust pipe 1 and furnace tail air inlet pipe 2
Gas circulator (production of Zhejiang Si Mingte fluid device Co., Ltd, model SMTD_XHJ_B100, SMTD_B_100 type of arranging in pairs or groups
Booster pump).
The above-mentioned semicontinuous boron nitride nano-tube of push boat type prepares the application method of furnace, comprising the following steps: (a) starts first
Electric control heating arrangement A sets temperature and heats to the burner hearth 8 of furnace body B;(b) burner fire door 3 and furnace tail fire door are then switched off
4, burner exhaust pipe 1 and furnace tail air inlet pipe 2 are opened, burner hearth 8 is vacuumized so that air is discharged as far as possible, then passes through furnace
Tail air inlet pipe 2 constantly conveys ammonia into burner hearth 8, and and then the ceramic boat for being paved with boron carbide powder is put into burner hearth 8
Carry out insulation reaction;(c) after the reaction was completed open burner C burner fire door 3, using push rod by ceramic boat be moved to furnace body B with
Cooling zone between furnace tail D is annealed, while another ceramic boat for being paved with boron carbide powder is put into burner hearth 8 and is carried out instead
It answers;(d) step (c) is repeated, the ceramic boat after annealing is taken out via the furnace tail fire door 4 of furnace tail D, and products therefrom is post-treated to be
Boron nitride nano-tube.
Further, ammonia flow velocity is 0.4-1.2L/min, and burner hearth heating rate is 4-10 DEG C/min.
Further, the ceramic boat for being paved with boron carbide powder is heated to 900-1400 DEG C, insulation reaction 3-15h.
Further, the post-processing includes the techniques such as pickling, washing, filtering, drying, detailed process are as follows: set product
8-16h is impregnated in the HCl solution of 10wt%-20wt%, then filters and is washed to filtrate and be in neutrality, and is finally placed in filter cake
8-16h is kept the temperature in 60-90 DEG C of environment.
Compared with prior art, the invention has the following advantages: (1) device is easy to operate, reaction raw materials and behaviour
It can easily be accommodated as technique, the product structure being prepared is rich and varied, is particularly suitable for industrialized production and application;
(2) gas-recycling plant between burner and furnace tail is set not only and ensure that reaction gas (NH3) obtain sufficiently
Effective use also contributes to regulation annealing reaction technological parameter, improves yield;
(3) device assembling is simple, and device security is high, stability is good, can not only effectively improve synthetic ratio and production energy
Power, and have height thermal control process integrated facilitates reaction temperature and accurately controls, adjusts and energy-saving;
(4) reactant is more advantageous to obtain purity more in specific reaction interval by heating device accuracy controlling reaction temperature
High target product, automatic heating is kept the temperature in the process, it is not necessary that driving a reaction object, external interference substantially reduce repeatedly;
(5) semi-continuous production, first ceramic boat are immediately transferred to recirculated water in burner hearth center after the reaction was completed
Cooling zone, second ceramic boat equipped with solid-phase reactant enters in burner hearth immediately is reacted, and last consignment of product is cooling
For next group product just insulation reaction (cooling product is still in ammonia atmosphere, can the reaction was continued), new product be anti-simultaneously
Having answered last consignment of product, cooling treatment is good, realizes seamless connection, greatly avoids device and repeats opening times and leave unused
Time realizes the purpose of continuous a large amount of synthesis BNNTs.
Detailed description of the invention
Fig. 1 is apparatus of the present invention overall structure diagram;
Fig. 2 is burner of the present invention or furnace tail recirculated water support cross-sectional view (lower half portion);
The XDR figure that Fig. 3 is BNNTs made from the embodiment of the present invention 2;
Fig. 4 is the raman spectrum of BNNTs made from the embodiment of the present invention 2;
The TEM figure that Fig. 5 is BNNTs made from the embodiment of the present invention 2.
Wherein, A- electric control heating arrangement, B- furnace body, C- burner, D- furnace tail, 1- burner exhaust pipe, 2- furnace tail air inlet pipe, 3-
Burner fire door, 4- furnace tail fire door, 5- stove head seal cover, 6- furnace tail seal closure, 7- furnace shell, 8- burner hearth, 9- furnace lining, 10- insulating layer,
11- burner table, 12- furnace tail table, 13- stainless steel tube, 14- boiler tube, 15-1 burner recirculated water support, 15-2 furnace tail recirculated water support, 16-
Flange, 17- stainless steel protection cover, 18- adjustment base.
Specific embodiment
To make those of ordinary skill in the art fully understand technical solution of the present invention and beneficial effect, below in conjunction with specific
Embodiment is further described.
Embodiment 1
Method using equipment synthesis inner wall smooth type boron nitride nano-tube as shown in Figure 1 provided by the invention is as follows:
Checking in advance ensures that equipment overall operation is good.Start electric control heating arrangement A, sets temperature and burner hearth 8 is carried out
Heating, 4-8 DEG C of heating rate/min.Burner fire door 3 and furnace tail fire door 4 are closed, burner exhaust pipe 1 and furnace tail air inlet pipe 2 are opened,
Vacuumizing and exhausting is carried out to burner hearth 8, ammonia, ammonia flow control are constantly then conveyed into burner hearth 8 by furnace tail air inlet pipe 2
System keeps pipeline gas circulator to be in and opens working condition in 0.4-1.0L/min.And then superfine boron carbide powder will be paved with
The ceramic boat at end, which is put into the burner hearth 8 of furnace body B, carries out insulation reaction, and 900-1350 DEG C of reaction temperature, soaking time 10-15h.Instead
The burner fire door 3 that burner C should be opened after the completion, is carried out the cooling zone that ceramic boat is moved between furnace body B and furnace tail D with push rod
Annealing, while another ceramic boat for being paved with boron carbide powder is put into burner hearth inside holding and is reacted.Abovementioned steps are repeated, even
It is continuous uninterruptedly to be reacted.During this period, the ceramic boat for completing annealing is taken out via the furnace tail fire door 4 of furnace tail D, products therefrom warp
After pickling, washing, filtering, drying process, the as boron nitride nano-tube of inner wall smooth.
Embodiment 2
Utilize the method and embodiment 1 of equipment synthesis slub type boron nitride nano-tube as shown in Figure 1 provided by the invention
It is substantially similar, the difference is that: heating rate is 6-10 DEG C/min, ammonia flow 0.6-1.2L/min, holding temperature 900-
1400 DEG C, soaking time 3-6h.XRD, Raman spectrum, tem analysis are carried out to slub type BNNTs made from embodiment 2, as a result
As in Figure 3-5.
It can be seen that, characteristic diffraction peak is all very clear from the feature XRD diffraction spectrogram of Fig. 3 BNNTs sample, illustrates sample
Product crystallization degree is preferable.Wherein the d value of characteristic diffraction peak is at 0.33492,0.21843,0.20786 and 0.16693nm, respectively
Corresponding to (002) of hexagonal boron nitride, (100), (101) and (004) crystal face.Thus calculating product lattice constant is a=
A=0.2504nm, c=0.6661nm in 0.2510nm, c=0.6766nm, with hexagonal boron nitride standard card JCPDF 73-2095
Substantially it is consistent, shows that product obtained is hexagonal boron nitride.Furthermore without finding the complete peak of B4C unreacted in XRD spectrum,
Show raw material B4C fully reacting.
Fig. 4 is the Raman spectrogram of BNNTs sample.1360cm-1Nearby there is absorption peak, with hexagonal boron nitride reticular structure
E2G in plane vibration mode is corresponding;Furthermore do not occur other characteristic absorption peaks in Raman spectrogram, show that sample composition is
High-purity hexagonal boron nitride.
It can be observed how nanotube in Bamboo-shaped cyclically-varying from the TEM photo of Fig. 5, nanometer pipe outer wall is smooth, internal
Hollow structure is taper, and outer diameter size is about 200nm.
Claims (10)
1. a kind of semicontinuous boron nitride nano-tube of push boat type prepares furnace, it is characterised in that this prepare furnace include electric control heating arrangement A,
Furnace body B, burner C, furnace tail D and push rod;Wherein electric control heating arrangement A is fixed on furnace body B, for being under controlled conditions furnace
Body B carries out heat temperature raising;It is provided with burner exhaust pipe (1) on burner C, furnace tail air inlet pipe (2) is provided on furnace tail D;Furnace
Head C and furnace tail D is connected by boiler tube (14) with the burner hearth (8) in furnace body B, and complete gas access way is formed;Push rod can
Burner hearth (8) by burner C and boiler tube (14) into burner B is interior, and the product in burner hearth is pushed between furnace tail D and furnace body B
Boiler tube in.
2. a kind of semicontinuous boron nitride nano-tube of push boat type as described in claim 1 prepares furnace, it is characterised in that: automatically controlled heating
Device A includes power control cabinet and heating element, and power control cabinet can control heating element and heat according to the program of setting to furnace body B
Heating, so that the temperature in burner hearth is stablized in setting value.
3. a kind of semicontinuous boron nitride nano-tube of push boat type as described in claim 1 prepares furnace, it is characterised in that: furnace body B packet
Furnace shell (7), burner hearth (8), furnace lining (9), insulating layer (10) are included, is arranged in and is enclosed with furnace lining the burner hearth (8) inside furnace body B Zhou Wei
(9), insulating layer (10) and furnace shell (7) are enclosed with outside furnace lining (9), furnace shell (7) is using the double-deck air-cooled structure.
4. a kind of semicontinuous boron nitride nano-tube of push boat type as described in claim 1 prepares furnace, it is characterised in that: burner C packet
Include burner exhaust pipe (1), burner fire door (3), stove head seal cover (5), burner table (11), burner recirculated water support (15-1);Burner
Exhaust pipe (1) is connected with boiler tube (14), for vacuumizing and being discharged the exhaust gas in burner hearth;Burner recirculated water support (15-1) socket
Behind boiler tube (14) outer surface, one end is fixed on burner table (11), and the other end is fixed on furnace body B;Stove head seal cover (5) will
In burner table (11), burner recirculated water support (15-1) are wrapped in and it is sealed;Burner exhaust pipe (1) setting is close in burner
On sealing cover (5), burner fire door (3) is arranged in boiler tube (14) end.
5. a kind of semicontinuous boron nitride nano-tube of push boat type as described in claim 1 prepares furnace, it is characterised in that: furnace tail D packet
Include furnace tail air inlet pipe (2), furnace tail seal closure (6), furnace tail fire door (4), furnace tail table (12), furnace tail recirculated water support (15-2);Furnace tail
Air inlet pipe (2) is connected with boiler tube (14), for conveying unstripped gas ammonia into burner hearth;Furnace tail recirculated water support (15-2) is socketed in
Boiler tube (14) outer surface forms cooling zone, and the one end furnace tail recirculated water support (15-2) is fixed on furnace tail table (12), and the other end is fixed
On furnace body B;Furnace tail table (12), furnace tail recirculated water support (15-2) are wrapped in interior and are sealed to it by furnace tail seal closure (6);
Furnace tail air inlet pipe (2) is arranged on furnace tail seal closure (6), and furnace tail fire door (4) is arranged in boiler tube (14) end.
6. a kind of semicontinuous boron nitride nano-tube of push boat type as described in claim 1 prepares furnace, it is characterised in that: followed in furnace tail
Ring water support (15-1) and the outer surface burner recirculated water support (15-2) are provided with stainless steel tube (13), stainless steel protection cover, in burner
Table (11) and furnace tail table (12) bottom are provided with adjustment base (18), furnace tail recirculated water support, burner recirculated water support and cooling water phase.
7. a kind of semicontinuous boron nitride nano-tube of push boat type as described in claim 1 prepares furnace, it is characterised in that: arranged in burner
Gas-recycling plant is additionally provided between tracheae (1) and furnace tail air inlet pipe (2).
8. the application method that the semicontinuous boron nitride nano-tube of push boat type described in claim 1 prepares furnace, which is characterized in that including with
Lower step:
(a) start electric control heating arrangement A first, set temperature and the burner hearth (8) of furnace body B is heated;
(b) it is then switched off burner fire door (3) and furnace tail fire door (4), burner exhaust pipe (1) and furnace tail air inlet pipe (2) are opened, to furnace
Thorax (8) is vacuumized so that air is discharged as far as possible, then constant defeated into burner hearth (8) by furnace tail air inlet pipe (2)
Ammonia is sent, the ceramic boat for being paved with boron carbide powder is and then put into the reaction of burner hearth (8) inside holding;
(c) the burner fire door (3) for opening burner C after the reaction was completed, using push rod by ceramic boat be moved to furnace body B and furnace tail D it
Between cooling zone anneal, while another ceramic boat for being paved with boron carbide powder is put into burner hearth (8) and is reacted;
(d) step (c) is repeated, the ceramic boat after annealing is taken out via the furnace tail fire door (4) of furnace tail D, and products therefrom is post-treated
As boron nitride nano-tube.
9. application method as claimed in claim 8, it is characterised in that: ammonia flow velocity is 0.4-1.2L/min, burner hearth heating speed
Rate is 4-10 DEG C/min, and the ceramic boat for being paved with boron carbide powder is heated to 900-1400 DEG C, insulation reaction 3-15h.
10. application method as claimed in claim 8, it is characterised in that: the post-processing specifically: place the product in
8-16h is impregnated in the HCl solution of 10wt%-20wt%, then filters and is washed to filtrate and be in neutrality, and is finally placed in filter cake
8-16h is kept the temperature in 60-90 DEG C of environment.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112857031A (en) * | 2020-12-31 | 2021-05-28 | 崇义章源钨业股份有限公司 | Oxidation reduction furnace |
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US20040092086A1 (en) * | 2001-03-28 | 2004-05-13 | Hitoshi Sakamoto | Film forming method and film forming device |
CN1840266A (en) * | 2006-01-26 | 2006-10-04 | 湖南凯丰新材料有限公司 | Preparation method and equipment for nano-grade superfine cobalt powder |
CN101885477A (en) * | 2010-07-15 | 2010-11-17 | 武汉工程大学 | Boron nitride nanotube synthesizer |
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