CN106276826B - A kind of system using fluidized-bed reactor synthesizing silicon nitride - Google Patents
A kind of system using fluidized-bed reactor synthesizing silicon nitride Download PDFInfo
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- CN106276826B CN106276826B CN201610952095.6A CN201610952095A CN106276826B CN 106276826 B CN106276826 B CN 106276826B CN 201610952095 A CN201610952095 A CN 201610952095A CN 106276826 B CN106276826 B CN 106276826B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/068—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with silicon
- C01B21/0682—Preparation by direct nitridation of silicon
Abstract
The present invention relates to a kind of system using fluidized-bed reactor synthesizing silicon nitride, including fluidized-bed reactor, nitrogen supply (NS) unit and silica flour feed unit, fluidized-bed reactor includes housing, the lower cavity of housing is used for nitrogen and nitridation reaction is carried out under fluidized state with silica flour, air supply opening and inlet are set on the shell wall of housing bottom, nitrogen supply (NS) unit includes the heater for heated nitrogen, the gas outlet of heater is connected with air supply opening, silica flour feed unit includes being used for the feeding barrel and Venturi feeder for containing silica flour, the discharging opening of feeding barrel is connected with the powder entrance of Venturi feeder, the discharging opening of Venturi feeder is connected with inlet, the discharging opening of case top is connected with reclaiming the cyclone separator of synthesizing silicon nitride.Said system makes silica flour under fluidized state and nitrogen reaction, synthesizes Si3N4Powder will not reunite caking, and can realize Si3N4The continuous production of powder.
Description
Technical field
The present invention relates to silicon nitride to synthesize field, and in particular to a kind of to be using fluidized-bed reactor synthesizing silicon nitride
System.
Background technology
Silicon nitride（Si3N4）Ceramics are a kind of advanced engineering ceramic materials, and the material has height at a room temperature and a high temperature
The features such as intensity, high rigidity, corrosion-resistant, wear-resistant and good heat shock resistance and mechanical shock performance, people are opened using it
Hair manufactured the mechanical components such as bearing, turbine blade, mechanical seal, and be widely used to metallurgy, aviation, petrochemical industry,
The industries such as machinery, electronics.Nearly two, 30 years Si3N4Quite favored and paid attention to.Therefore, high quality, the Si of low cost are manufactured3N4Powder
End, it has also become in industry the problem of common concern.
The preparation method of silicon nitride powder has a variety of, is silica flour direct nitridation method, SiO respectively2Carbothermic method, chemical gaseous phase
Method and thermal decomposition method etc..Various preparation methods, there is its existing value and continually develop the reasons why progressive.Wherein silica flour is direct
Nitriding is that one kind prepares Si using combustion synthesis technology3N4The method of powder.In this method, scholars, researcher
Numerous studies have been carried out, many papers has been delivered and has also applied for many patents, it is therefore intended that exploitation one kind is continuously synthesizing to Si3N4
Method.
Silica flour direct nitridation method prepares Si3N4It is current preparation Si3N4The main method of powder, but this method is main
Shortcoming is the Si of synthesis3N4Easily reunite, can lump, therefore, the Si generated after reaction3N4Need to grind, homogenize；This method
Further drawback be production process be interruption, it is discontinuous.It is therefore desirable to provide a kind of new Si3N4Powder preparation method and
System.
The content of the invention
The primary and foremost purpose of the present invention is just to provide a kind of system using fluidized-bed reactor synthesizing silicon nitride, and it can be effective
Solve the above problems, make silica flour under fluidized state and nitrogen reacts, synthesize Si3N4Powder will not reunite caking, and can realize
Si3N4The continuous production of powder.
To achieve the above object, present invention employs following technical scheme：
A kind of system using fluidized-bed reactor synthesizing silicon nitride, including fluidized-bed reactor, nitrogen supply (NS) unit with
And silica flour feed unit, it is characterised in that：Fluidized-bed reactor includes housing, and the lower cavity of housing is used for nitrogen and existed with silica flour
Nitridation reaction is carried out under fluidized state, sets air supply opening and inlet, nitrogen supply (NS) unit to include on the shell wall of housing bottom
For the heater of heated nitrogen, the gas outlet of heater is connected with air supply opening, and silica flour feed unit includes being used to contain
The feeding barrel and Venturi feeder of silica flour are filled, the discharging opening of feeding barrel is connected with the powder entrance of Venturi feeder, text
The discharging opening of feeder is connected with inlet in mound, the cyclone separator of the discharging opening and recovery synthesizing silicon nitride of case top
It is connected.
Further scheme is：
Also include filter and air-introduced machine, cyclone separator top outlet inlet is connected with filter, the air-out of filter
Mouthful it is connected with air-introduced machine, the air outlet of air-introduced machine, which be divided to the gas access that two transportation work styles do not connect Venturi feeder and heated, to be filled
The air inlet put.
Pipe heat exchanger A is provided with the upper chamber of housing, pipe heat exchanger A cold fluid inlet and venturi feed
The discharging opening of device is connected, and pipe heat exchanger A cold fluid outlet is connected with inlet.
Pipe heat exchanger C is provided with the upper chamber of housing, pipe heat exchanger C cold fluid inlet is connected with source nitrogen
Connect, pipe heat exchanger C cold fluid outlet is connected with the air inlet of heater.
Pipe heat exchanger B, pipe heat exchanger B cold fluid inlet and going out for air-introduced machine are provided with the upper chamber of housing
Air port is connected, and pipe heat exchanger B cold fluid outlet is connected with the air inlet of heater.
Pipe heat exchanger A, B, C are arranged in order setting from the bottom to top in the upper chamber of housing.
The air supply pipe of row of horizontal arrangement is provided with air supply opening, air supply pipe is extended in housing cavity, and herein at pipe
Venthole is set, intracavitary is provided with the baffle plate of arrangement shape arrangement in housing bottom, and baffle plate founds shape and is fixed on the internal face of housing,
The separated arrangement in shell bottom of the lower end and housing of baffle plate, air supply pipe arrangement corresponding with the lower end flush of baffle plate, baffle plate setting
Between two adjacent air supply pipes.
Venthole includes first and second venthole, and pipe shaft of first and second venthole along air supply pipe is arranged at intervals in pairs, first,
Gas flow at two ventholes is obliquely and is respectively directed on the outside of the two of air supply pipe, the center line and lead of the first venthole
The angle of vertical line is 30 °, and the center line of the second venthole and the angle of plumb line are 45 °, and the first venthole is arranged on air supply pipe
On the tube wall of upper close inlet side.
The upper side edge portion of baffle plate is not connected with case inside wall, is suspension shape；The downside edge and housing of baffle plate
The separated arrangement of inner side wall surface, the distance between they are 25-50mm, and are connected with the air supply pipe outside equipment, baffle plate two
Side portion and case inside wall Joint.
Nitrogen flow control valve A and fresh Nitrogen Control Units are set on the pipeline that pipe heat exchanger C is connected with source nitrogen,
Fresh Nitrogen Control Units regulation and control nitrogen flow control valve A running status；The air outlet of air-introduced machine and Venturi feeder gas
Nitrogen flow control valve B is set on the connecting pipe between entrance and send silica flour Nitrogen Control Units, send silica flour nitrogen control dress
Put regulation and control nitrogen flow control valve B running status；Heater is connected with temperature control equipment, temperature control equipment regulation and control
The outlet nitrogen temperature of heater（With nitrogen temperature speed）；The discharge outlet of case top sets pressure tester A（Air pressure）
With temperature measuring equipment A, temperature measuring equipment B is set between pipe heat exchanger A, B, temperature measuring equipment C, pipe are set between pipe heat exchanger B, C
Pressure tester B and temperature measuring equipment D is set between formula heat exchanger C and baffle plate, between adjacent screen clamping form what is passed through for material
Passage, the upper end of passage set temperature measuring equipment E, and the lower end of passage sets temperature measuring equipment F, pipe heat exchanger B cold fluid inlet
Pressure tester C and temperature measuring equipment G, pipe heat exchanger A and heater are set on the pipeline being connected with the air outlet of air-introduced machine
Temperature measuring equipment H is set on the pipeline being connected, and has pipeline to be connected.
Use the method for said system synthesizing silicon nitride for：
20~40mm of particle mean size Si powder is added with standby in feeding barrel, the nitrogen stream at opening source nitrogen gas outlet
Control valve A, when pressure tester B detects that pressure is 10~20mmH2During O, the sealing of whole device is checked, is then carried out
Warm-up operation；
Warm-up operation includes：Start heater（Make the outlet N of heater by temperature control equipment2Temperature rise is 10
~20 DEG C/min）, when regulation and control heater to outlet temperature is 200 DEG C, start air-introduced machine, open nitrogen flow control valve B, and
By sending silica flour Nitrogen Control Units to control N2Flow is in 20~120L/h（Most of N of air-introduced machine outlet2Pass through pipe type heat transfer
Device B and heater return to housing bottom, and that goes round and begins again circulate）.
After warm-up operation terminates, the discharge valve A that feeding barrel discharge outlet is set is opened, Si powder is passed through Venturi feeder
Participate in reacting into fluidized-bed reactor bottom；Meanwhile accelerate the programming rate of heater, until the outlet temperature of heater
Spend for 1250~1380 DEG C, and maintained by the outlet temperature of temperature control equipment heater in the interval range,
Then big discharge valve A is gradually opened, the feed rate for making Si powder is 50~100kg/h.
Because the Direct-Nitridation reaction of Si powder is an exothermic reaction, there is heat releasing during the course of the reaction, reactant can be made
Expect that system temperature rises 15~30 DEG C.To make reaction temperature is unlikely too high to influence Si3N4Product quality, reaction temperature control exist
1300~1380 DEG C（Temperature measuring equipment D is measured）.Control method is：The nitrogen hand set by each air supply pipe inlet end of adjustment control
The aperture size of dynamic regulating valve.
The Si of nitridation reaction generation3N4, the Si that can largely be opened up from housing3N4Discharging opening is discharged, a small amount of thin Si3N4Powder
The high temperature carrier gas N that can be reacted with fluidization2Continue to rise, carrier gas N2Partial heat is passed in pipe heat exchanger A, B, C
Cold fluid, the temperature of itself can decline.The carrier gas that temperature has declined enters cyclone separator, the thin Si separated3N4Powder, lead to
The discharging opening discharge of whirlwind separator bottom is crossed, the discharge outlet of cyclone separator bottom sets discharge valve B, separates meticulous Si3N4
The carrier gas N of powder2Filtered into filter, enter back into high temperature draught fan and participate in circulation.
The production system provided in the present invention, silica flour is reacted under fluidized state with nitrogen, synthesizes Si3N4Powder.Due to
Solid particle is suspended in nitrogen medium, and gas-particle two-phase contact surface area is big, is advantageous to accelerate heat transfer, mass transfer and was chemically reacted
The speed of journey.Solid particle is in strong agitation state, and reactor temperature is easy to remain uniform, beneficial to raising sintetics
Quality, and because silicon nitride synthetic reaction is an exothermic reaction, this partial heat can be reclaimed back by appropriate heat exchange mode
Come, for the heat consumed needed for synthetic reaction.Important technical parameter in reactor all shown by computer and
Control, enable nitridation reaction device long-term, steady, safety, low consumption, it is easy to control continuously run, produce that cost is low, quality meets
It is required that Si3N4Powder.
Brief description of the drawings
Fig. 1 is the structural representation of the present invention；
Fig. 2 is the structural representation of fluidized-bed reactor；
Fig. 3 is Fig. 2 A-A cross section structure diagrams；
Fig. 4 is Fig. 2 B-B cross section structure diagrams；
Fig. 5 is the schematic diagram in the section of air supply pipe.
Embodiment
In order that objects and advantages of the present invention are more clearly understood, the present invention is carried out specifically with reference to embodiments
It is bright.It should be appreciated that following word only to describe the present invention one or more of specific embodiments, not to the present invention
The protection domain specifically asked carries out considered critical.
The technical scheme that the present invention takes is as shown in Figure 1,2,3, 4, a kind of using fluidized-bed reactor synthesizing silicon nitride
System, including fluidized-bed reactor 11, nitrogen supply (NS) unit and silica flour feed unit, fluidized-bed reactor 11 include housing,
The lower cavity of housing is used for nitrogen and nitridation reaction is carried out under fluidized state with silica flour, sets and supplies on the shell wall of housing bottom
Gas port and inlet, nitrogen supply (NS) unit include the heater 17 for heated nitrogen, the gas outlet of heater 17 and confession
Gas port is connected, and silica flour feed unit includes being used for the feeding barrel 15 and Venturi feeder 16 for containing silica flour, feeding barrel 15
Discharging opening is connected with the powder entrance of Venturi feeder 16, and the discharging opening of Venturi feeder 16 is connected with inlet,
The discharging opening of case top is connected with reclaiming the cyclone separator 12 of synthesizing silicon nitride.
Further scheme is：Also include filter 13 and air-introduced machine 14, the top outlet inlet of cyclone separator 12 and filtering
Device 13 is connected, and the air outlet of filter 13 is connected with air-introduced machine 14, and the air outlet of air-introduced machine 14 is divided to two transportation work styles not connect text
The air inlet of the gas access of feeder 16 and heater 17 in mound.Pipe heat exchanger is provided with the upper chamber of housing
A, pipe heat exchanger A cold fluid inlet are connected with the discharging opening of Venturi feeder 16, and pipe heat exchanger A cold fluid goes out
Mouth is connected with inlet.Be provided with pipe heat exchanger C in the upper chamber of housing, pipe heat exchanger C cold fluid inlet with
Source nitrogen is connected, and pipe heat exchanger C cold fluid outlet is connected with the air inlet of heater 17.The upper chamber of housing
Pipe heat exchanger B is inside provided with, pipe heat exchanger B cold fluid inlet is connected with the air outlet of air-introduced machine 14, pipe type heat transfer
Device B cold fluid outlet is connected with the air inlet of heater 17.Pipe heat exchanger A, B, C in the upper chamber of housing by
Under supreme be arranged in order setting.The air supply pipe 116 of row of horizontal arrangement is provided with air supply opening, air supply pipe 116 extends to housing
Interior intracavitary, pipe shaft set venthole, and intracavitary is provided with the baffle plate 115 of arrangement shape arrangement in housing bottom, and baffle plate 115 founds shape and fixed
On the internal face of housing, the separated arrangement in shell bottom of the lower end and housing of baffle plate 115, under air supply pipe 116 and baffle plate 115
Hold flush is corresponding to arrange, baffle plate 115 is arranged between two adjacent air supply pipes 116.Venthole includes first and second venthole,
Pipe shaft of first and second venthole along air supply pipe 116 is arranged at intervals in pairs, and the gas flow at first and second venthole is oblique
Two outside that is lower and being respectively directed to air supply pipe 116, the center line of the first venthole and the angle of plumb line are 30 °, the second outlet
The center line in hole and the angle of plumb line are 45 °, and the first venthole is arranged on air supply pipe 116 close to the tube wall of inlet side
On.
The A side portions of baffle plate 115 are connected with case inside wall, and B side portions and the case inside wall of baffle plate 115 are in
Separate shape arrangement, A side portions and B side portions are that baffle plate 115 founds shape two edge positioned opposite, the gas stream in air supply pipe 116
A side portions are pointed to for B side portions.On the pipeline that pipe heat exchanger C is connected with source nitrogen set nitrogen flow control valve A and
Fresh Nitrogen Control Units, fresh Nitrogen Control Units 21 regulate and control nitrogen flow control valve A running status；The air outlet of air-introduced machine 14
Nitrogen flow control valve B is set on the connecting pipe between the gas access of Venturi feeder 16 and send silica flour nitrogen control dress
Put, send silica flour Nitrogen Control Units 22 to regulate and control nitrogen flow control valve B running status；Heater 17 and temperature control equipment
23 are connected, and temperature control equipment 23 regulates and controls the outlet nitrogen temperature of heater 17（With nitrogen temperature speed）；Case top
Discharge outlet pressure tester A is set（Air pressure）With temperature measuring equipment A, temperature measuring equipment B, tubular type are set between pipe heat exchanger A, B
Temperature measuring equipment C is set between heat exchanger B, C, pressure tester B and temperature measuring equipment D is set between pipe heat exchanger C and baffle plate 115,
Clamping forms the passage passed through for material between adjacent screen 115, and the upper end of passage sets temperature measuring equipment E, and the lower end of passage is set
Put temperature measuring equipment F, set pressure measurement to fill on the pipeline that pipe heat exchanger B cold fluid inlet is connected with the air outlet of air-introduced machine 14
C and temperature measuring equipment G are put, sets temperature measuring equipment H, A and 17 to have pipeline on the pipeline that pipe heat exchanger A is connected with heater 17
It is connected.
Si powder is added in the feeding barrel 15 in said system in case nitridation reaction is used, discharged as long as starting feeding barrel 15
The star charging valve and nitrogen flow control valve B set at mouthful, it is possible to reactor 11 plus Si powder raw materials.N2Pass through fresh nitrogen
Control device 21 regulates and controls, and by being passed through N to reactor 11 after the heating of heater 172.Into the N of the bottom of reactor 112And Si
Powder, nitridation reaction is carried out in fluidized state, reaction institute liberated heat will be passed to reaction product, mainly Si3N4Flowed with rising
The carrier gas N of change effect2, raise its temperature.Pipe heat exchanger A of the reaction product by three superpositions thereon（Label in Fig. 2
113 part）, pipe heat exchanger B（The part of label 112 in Fig. 2）, pipe heat exchanger C（The part of label 111 in Fig. 3）, will
Partial heat is passed to the cold fluid with its heat exchange.And the temperature of itself will decline, while the portion entrained by it
Divide product Si3N4The bottom of reactor 11 will be dropped to, with finished product Si3N4Reactor 11 is discharged by finished product discharge nozzle.This part
So-called reaction product is carrier gas in fact, and the effect of carrier gas is to aid in raw material Si powder and product Si3N4Powder carries out fluidised.Carry
Gas is when by cyclone separator 12, the thin Si of the overwhelming majority therein3N4All reclaim in the bottom of cyclone separator 12, by beating
Open the star valve at the bottom discharge mouth of cyclone separator 12, thin Si3N4Can reclaims.Arranged by the top of cyclone separator 12
The carrier gas gone out can contain a small amount of superfine Si3N4, high temperature draught fan 14 is entered by the carrier gas of filter 13.The load of substantially free of impurities
Gas is divided into two bursts of outflows after the pressurization of air-introduced machine 14, and one a small amount of carrier gas is used as the medium of conveying Si powder；One is big
Pipe heat exchanger B, and the N with being come out in pipe heat exchanger B, C are passed through in the carrier gas of amount2One is converged into, into heater 17（Electricity
Heating furnace）, it is heated to required temperature, and the bottom of Returning reactor 11.N of the small part needed for as reaction2, it is most of to make
For fluidised carrier gas.
Reaction concentrates on the bottom of reactor 11, and the housing cross-sectional of the bottom of reactor 11 is rectangle, is set in length direction
5 chambers will be divided into by putting the baffle plate 115 of vertical arrangement arrangement inside reactor 11.The downside edge of baffle plate 115 and the shell of reactor 11
Certain gap is left between bottom, enables powder granule by room by drawing off reactor 11 finally by outlet.This structure
Feature is, N2Each lead into each room, the logical N of each room2Speed can adjust, thus the reaction temperature of 11 each room of reactor
It can be adjusted, residence time of the material in reactor 11 can suitably be adjusted.N2Divided by 5 nitrogen air supply pipes 116
5 rooms are not passed through, carry out the fluidization of powder.
Heat-exchange system concentrates on the top of reactor 11, is respectively from top to bottom pipe heat exchanger A, B, C according to arrangement, this three
Individual heat exchanger-type is similar to food steamer, is superimposed upon the top of reactor 11, and composition one has response function, has the synthesis of heat exchange function anti-again
Answer device 11.Pipe heat exchanger A hot-fluids side is the circulating carried of fluidized-bed reaction, and cold flow side is Si powder and air-flow conveying Si powder N2's
Mixture.Pipe heat exchanger B hot-fluids side is the circulating carried of fluidized-bed reaction, and cold flow side is fluidized carrier gas.Pipe heat exchanger C heat
Stream side is the circulating carried of fluidized-bed reaction, and cold flow side is fresh N2.Si of the Product recycling essentially from reactor 113N4Particle,
And fluidized reaction carrier gas N2The entrained thin Si reclaimed by cyclone separator 1273N4Particle.
Control system include fresh Nitrogen Control Units 21, send silica flour Nitrogen Control Units 22, temperature control equipment 23 and
The manual control systems such as some temperature, pressure instruction.
The structure of reactor 11 is broadly divided into four part compositions：One is lower house a；Two be middle housing b, and three be upper casing
Body c, its top is top cover d.Lower house a is that three housings are formed by connecting.Its housing upper is cuboid upper housing portion, middle part
It is that water chestnut platform shape housing section, bottom are cuboid bottom housing parts, the top of water chestnut platform shape housing section and cuboid upper housing portion bottom connect
Connecing, the bottom of water chestnut platform shape housing section connects with the top of cuboid bottom housing part, and lower house a upper surface is flange connector,
Fastener bolt and nut and middle housing b bottom adpting flange connection sealed to each other can be passed through.Lower house a inside is welded with pipe
Formula heat exchanger A, pipe heat exchanger A heat exchanger tube pass through lower house a side wall, and its top is the import of cold fluid, and its underpart is
The outlet of cold fluid.In the middle part of water chestnut platform shape housing section pressure gauge connection and thermometer boss are welded with shell wall.Lower house a bottom is
Flange connector, it can be tightly connected by fastener bolt and nut and bottom plate.Opened in the rectangular long side in its underpart cross section
There are 5 adapter holes, being gone here and there in hole has N2Air supply pipe 5.Every pipe opens 5 device to hole as shown in figure 5, totally 10 holes, aperture Ф
2mm, it is equal per the distance between device to hole, it is therefore an objective to allow N2Distribution is as far as possible uniform.There is the conveying N for carrying Si powder its underpart2's
Import, finished product Si is additionally provided with the middle of its underpart3N4The outlet of powder.Below the inside of reactor 11,4 pieces are additionally provided with
Vertical baffle 115, the distance between baffle plate 115 and bottom plate are between 25~50mm, and the height of baffle plate 115 is between 40~90mm.
Side wall, baffle plate 115 altitude range in it is upper and lower respectively open a thermometer boss as shown in Fig. 2 so as to test temperature, can enter
Row regulation.
Middle housing b is a cuboid, and top is welded with flange connector, can pass through fastener bolt and nut and upper shell c
Lower flange be tightly connected.Middle housing b inside is welded with pipe heat exchanger B, and pipe heat exchanger B top sets entering for cold fluid
Mouthful, pipe heat exchanger B bottom sets the outlet of cold fluid, and one is provided with the side wall of the middle housing b on the downside of pipe heat exchanger B
Individual thermometric interface.
Upper shell c is a cuboid, and cuboid side wall upper part is welded with flange connector, can pass through fastener bolt and nut
Connected with top cover d flange seal.Upper shell c inside is welded with pipe heat exchanger C, and pipe heat exchanger C top sets cold flow
The import of body, pipe heat exchanger C bottom set the outlet of cold fluid, in the side wall of the upper shell c on the downside of pipe heat exchanger C
It is provided with a thermometric interface.
Top cover d is a water chestnut taper, and a thermometer boss and a pressure test interface are provided with its side.
Specific production operation is：
The Si powder that particle mean size is 20~40mm is added into feeding barrel 15 with standby.
High-purity N2Whole reaction unit is continuously entered by nitrogen flow control valve A, when the inner chamber of reactor 11
Display pressure is 10~20mmH2During O, the seal point of whole device is conscientiously checked, when inspection processing terminates, all seal points are all
Do not leak and whole device is intact, device can enters warm-up phase.
Start heater 17, by operation temperature control device 23, heater 17 is exported N2Temperature rise is 10~20
℃/min.When the outlet temperature of heater 17 is 200 DEG C, starts high temperature draught fan 14, open air-flow supplying nitrogen flow control
Valve B processed, and by giving silica flour Nitrogen Control Units 22 to regulate and control N2Flow is in the big portion that 20~120L/h, high temperature draught fan 14 are exported
Divide N2Pipe heat exchanger B and the bottom of 17 Returning reactor of heater 11 by the top of reactor 11, the progress to go round and begin again
Circulation.
About 10~20min after whole device is warm-up to be terminated, start star charging and cut down, a small amount of Si powder is added by venturi
Glassware 16 enters the bottom of reactor 11 and participates in reaction.Meanwhile accelerate the programming rate of heater 17, about 30~50 DEG C/min,
Until the outlet temperature of heater 17 is 1250~1380 DEG C, and the temperature is controlled by temperature control equipment 23.When the temperature
After degree can be controlled effectively, gradually open big star charging and cut down, the flow for making Si powder is 50~100kg/h.Because the direct nitrogen of Si powder
It is an exothermic reaction to change reaction, there is heat releasing during the course of the reaction, and reaction mass system temperature can be made to rise 15~30 DEG C.For
Make reaction temperature unlikely too high and influence Si3N4Product quality, reaction temperature are controlled at 1300~1380 DEG C.Control method is：It is logical
Overregulate the aperture size that five inlet ends of air supply pipe 116 of control set nitrogen manual modulation valve.
The Si of nitridation reaction generation3N4, largely can be from Si3N4Discharging opening is discharged, a small amount of thin Si3N4Powder can be with fluidization
The high temperature carrier gas N of reaction2Continue to rise.Carrier gas N2Partial heat is passed to pipe heat exchanger A（The portion of label 113 in Fig. 2
Part）, pipe heat exchanger B（The part of label 112 in Fig. 2）, pipe heat exchanger C（The part of label 111 in Fig. 3）In cold flow
Body, the temperature of itself can also decline.The carrier gas that temperature has declined enters cyclone separator 12, the thin Si separated3N4Powder passes through
Bottom discharge mouth is discharged, and separates meticulous Si3N4The carrier gas N of powder2Filtered into filter 13, enter back into high temperature draught fan 14
Participate in circulation.
As a result of technical scheme as described above, reactant Si powder and N in the present invention2Amount can control, fluidised form
Change carrier gas N2Flow also can control, reaction temperature and reaction time can be adjusted within the specific limits, so continuous production
It is possible, and product quality is easily guaranteed that.
Other heat exchanger and reactor 11 are combined as a whole, and the chemical energy of material can be converted into heat energy to greatest extent,
Heat loss required for supply response, the energy consumption of production is reduced to a certain extent.This energy-saving scheme is desirable.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, after content described in the present invention is known, under the premise without departing from the principles of the invention, it can also be made some
Equal conversion and replacement, these, which convert and substituted on an equal basis, also should be regarded as belonging to protection scope of the present invention.
Claims (7)
1. a kind of system using fluidized-bed reactor synthesizing silicon nitride, including fluidized-bed reactor, nitrogen supply (NS) unit and
Silica flour feed unit, it is characterised in that：Fluidized-bed reactor includes housing, and the lower cavity of housing is flowing for nitrogen with silica flour
Nitridation reaction is carried out under state state, air supply opening and inlet are set on the shell wall of housing bottom, nitrogen supply (NS) unit includes using
In the heater of heated nitrogen, the gas outlet of heater is connected with air supply opening, and silica flour feed unit includes being used to contain
The feeding barrel and Venturi feeder of silica flour, the discharging opening of feeding barrel are connected with the powder entrance of Venturi feeder, literary mound
In the discharging opening of feeder be connected with inlet, the discharging opening of case top and the cyclone separator phase for reclaiming synthesizing silicon nitride
Connection；
Also include filter and air-introduced machine, cyclone separator top outlet inlet is connected with filter, the air outlet of filter with
Air-introduced machine is connected, and the air outlet of air-introduced machine divides the gas access that two-way connects Venturi feeder respectively and heater
Air inlet；
It is provided with pipe heat exchanger A in the upper chamber of housing, pipe heat exchanger A cold fluid inlet and Venturi feeder
Discharging opening is connected, and pipe heat exchanger A cold fluid outlet is connected with inlet.
2. the system according to claim 1 using fluidized-bed reactor synthesizing silicon nitride, it is characterised in that：Housing it is upper
Pipe heat exchanger C is provided with portion's cavity, pipe heat exchanger C cold fluid inlet is connected with source nitrogen, pipe heat exchanger C's
Cold fluid outlet is connected with the air inlet of heater.
3. the system according to claim 2 using fluidized-bed reactor synthesizing silicon nitride, it is characterised in that：Housing it is upper
Pipe heat exchanger B is provided with portion's cavity, pipe heat exchanger B cold fluid inlet is connected with the air outlet of air-introduced machine, tubular type
Heat exchanger B cold fluid outlet is connected with the air inlet of heater.
4. the system according to claim 3 using fluidized-bed reactor synthesizing silicon nitride, it is characterised in that：Pipe type heat transfer
Device A, B, C are arranged in order setting from the bottom to top in the upper chamber of housing.
5. the system according to claim 1 using fluidized-bed reactor synthesizing silicon nitride, it is characterised in that：At air supply opening
The air supply pipe of row of horizontal arrangement is provided with, the outlet side of air supply pipe is extended in housing cavity, and the pipe in housing cavity
Setting venthole is in, intracavitary is provided with the baffle plate that arrangement shape is arranged in housing bottom, and baffle plate founds the inwall that shape is fixed on housing
On face, the separated arrangement in shell bottom of the lower end and housing of baffle plate, air supply pipe arrangement corresponding with the lower end flush of baffle plate, baffle plate
It is arranged between two adjacent air supply pipes.
6. the system according to claim 5 using fluidized-bed reactor synthesizing silicon nitride, it is characterised in that venthole bag
First and second venthole is included, pipe shaft of first and second venthole along air supply pipe is arranged at intervals in pairs, the gas at first and second venthole
Flow direction is obliquely and is respectively directed to two outsides of air supply pipe, and the center line of the first venthole and the angle of plumb line are 30 °,
The center line of second venthole and the angle of plumb line are 45 °, and the first venthole is arranged on air supply pipe close to inlet side
Tube wall on.
7. the system according to claim 5 using fluidized-bed reactor synthesizing silicon nitride, it is characterised in that pipe type heat transfer
Nitrogen flow control valve A and fresh Nitrogen Control Units are set on the pipeline that device C is connected with source nitrogen, and fresh Nitrogen Control Units are adjusted
Control nitrogen flow control valve A running status；Connecting tube between the air outlet of air-introduced machine and Venturi feeder gas access
Nitrogen flow control valve B is set on road and send silica flour Nitrogen Control Units, send silica flour Nitrogen Control Units to regulate and control nitrogen flow control
Valve B processed running status；Heater is connected with temperature control equipment, and temperature control equipment regulates and controls the outlet nitrogen of heater
Temperature degree；The discharge outlet of case top sets pressure tester A and temperature measuring equipment A, sets thermometric to fill between pipe heat exchanger A, B
B is put, temperature measuring equipment C is set between pipe heat exchanger B, C, pressure tester B and thermometric dress are set between pipe heat exchanger C and baffle plate
Put D, between adjacent screen clamping form the passage passed through for material, the upper end of passage sets temperature measuring equipment E, and the lower end of passage is set
Temperature measuring equipment F is put, pressure tester is set on the pipeline that pipe heat exchanger B cold fluid inlet is connected with the air outlet of air-introduced machine
C and temperature measuring equipment G, temperature measuring equipment H is set on the pipeline that pipe heat exchanger A is connected with heater.
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| CN109422251A (en) * | 2017-08-22 | 2019-03-05 | 新特能源股份有限公司 | Silicon powder for fluidized reaction and preparation method thereof, silicon nitride and its production method |
| CN109467063A (en) * | 2017-09-07 | 2019-03-15 | 江苏中能硅业科技发展有限公司 | The fluidized-bed reactor and its apparatus system and method for production silicon nitride |
| CN108059166B (en) * | 2017-12-27 | 2021-04-30 | 江苏乐园新材料集团有限公司 | Preparation method of fluctuation type silicon carbide and heating device thereof |
| CN108128777B (en) * | 2017-12-27 | 2021-07-30 | 江苏乐园新材料集团有限公司 | Dynamic suspension friction type silicon carbide preparation method and heating device thereof |
| CN108622864B (en) * | 2018-04-13 | 2019-10-29 | 浙江东瓷新材料有限公司 | A kind of reaction system for synthesizing silicon nitride powder |
| CN108609589B (en) * | 2018-04-13 | 2020-01-03 | 浙江东瓷新材料有限公司 | Silicon nitride powder suspension reactor |
| CN108609590B (en) * | 2018-04-19 | 2019-10-29 | 浙江东瓷新材料有限公司 | A kind of beta-silicon nitride powder production line |
| CN108610054A (en) * | 2018-05-21 | 2018-10-02 | 北京中材人工晶体研究院有限公司 | A kind of preparation method of high-purity gamma-ALON powder |
| CN110204342B (en) * | 2019-06-10 | 2020-06-30 | 宁夏秦氏新材料有限公司 | Preparation method of sedimentation type self-propagating aluminum nitride |
| CN115432677B (en) * | 2021-06-04 | 2024-03-22 | 中国科学院过程工程研究所 | System and method for preparing high-quality silicon nitride powder by impinging stream coupling fluidized bed |
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