CN207619027U - A kind of lift bed beta-silicon nitride powder preparation system - Google Patents
A kind of lift bed beta-silicon nitride powder preparation system Download PDFInfo
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Abstract
The utility model provides a kind of lift bed beta-silicon nitride powder preparation system, and wherein silica flour for being periodically fed through lift bed reactor bottom by silica flour storage tank；Heater is used to after low temperature nitrogen is heated to the first preset temperature range export to lift bed reactor bottom；Into lift bed reactor bottom silica flour and nitrogen flow from bottom to top during react generate beta-silicon nitride powder, and react after tail gas export to bag hose；Bag hose is used to carry out gas solid separation processing to tail gas after reaction, and the material position of the solid particle in its cavity is when reaching preset height, the solid particle isolated is exported to lift bed reactor bottom, to continue to participate in reaction, and the gas isolated directly is vented；The content that lift bed reactor is additionally operable to the beta-silicon nitride powder in it stops reaction when reaching preset value, and exports and be discharged from reactor bottom.The utility model can improve production efficiency and reduce requirement of the reaction process to silica flour, it is easy to accomplish industrial applications.
Description
Technical field
The utility model is related to beta-silicon nitride powder production technical fields, and in particular to a kind of lift bed beta-silicon nitride powder preparation
System.
Background technology
Silicon nitride has that high mechanical strength, self-lubricating, thermal stability be good, good chemical stability, in high temperature, height
In particular job environment such as speed, strong corrosive medium and high abrasion, have a wide range of applications.Silicon nitride molecular formula is Si3N4, it is one
Kind has α-Si with the compound of Covalent bonding together3N4、β-Si3N4、γ-Si3N4Three kinds of phases are kinetically being easier to generate α
Phase, undergoes phase transition producible thermodynamically stable β phases at high temperature, and γ phases could only synthesize under high pressure and high temperature.Its
In, since α phases are more active, it is easy to sinter product into, therefore commercial Application is with α-Si3N4Based on.
There are many phases for silicon nitride, and reaction temperature is different, will generate out of phase beta-silicon nitride powder, therefore the control of temperature
System directly affects the quality of beta-silicon nitride powder.But silicon powder nitride is exothermic process, if the heat generated in reaction process is not
Can remove in time can cause hot-spot phenomenon, and the α phase silicon nitrides generated is caused to undergo phase transition, and be generated it also occur that silica flour melts
The phenomenon that flowing silicon.Meanwhile silicon reacted with nitrogen after can generate the surface that silicon nitride film is wrapped in silicon powder particle, hinder nitrogen and silicon
The further contact of element influences the further progress of reaction, therefore in order to reduce the resistance of nitrogen infiltration, prepares silicon nitride powder
The silicon powder particle grain size very little of body, generally 10-20 μm.
The technology that traditional direct nitridation method prepares silicon nitride mainly uses fixed bed reactors, the technology to pass through in raw material
A certain proportion of beta-silicon nitride powder is added in silica flour increases the indifferent gas such as a certain proportion of argon gas as diluent or in nitrogen
Body, to reduce the intensity of reaction process, prevent in reaction process occur overtemperature the problem of, but the reaction time of this method compared with
Long, efficiency is low, and production cost is high.
It, the advantages that gas, solid phase interface product are big, and reaction rate is fast, can be in view of fluid bed has heat transfer, mass transfer rate high
Solve the problems, such as that non-uniform temperature during silicon powder nitride, reaction rate are slow, Some Enterprises and colleges and universities attempt to use fluidized bed process
Prepare beta-silicon nitride powder.However, during preparing silicon nitride using fluidized bed process, if using bulky grain silica flour, although can
To realize fluidisation, but silica flour reacted with nitrogen can in the Surface Creation silicon nitride layer of silica flour, can prevent silica flour and nitrogen into
Single step reaction；If using small particle silica flour, although the resistance of nitridation reaction can be reduced, solid particle is too thin, it is difficult to
Fluidisation.As it can be seen that fluidized bed process is to the more demanding of silica flour, it is difficult to realize industrial applications.
Therefore, urgently there is one kind and can improve production efficiency and reduce reaction process to want silica flour in the prior art
It asks, it is easy to accomplish the silicon nitride technology of preparing of industrial applications.
Utility model content
Technical problem to be solved in the utility model is to provide one kind for the drawbacks described above in the presence of the prior art
Production efficiency can be improved and reduce requirement of the reaction process to silica flour, it is easy to accomplish the lift bed of industrial applications nitrogenizes
Silicon powder preparation system.
Technical solution is used by solving the utility model technical problem：
The utility model provides a kind of lift bed beta-silicon nitride powder preparation system comprising silica flour storage tank, lift bed reaction
Device, heater and bag hose,
Silica flour for being periodically fed through lift bed reactor bottom by the silica flour storage tank；
The heater is used to after low temperature nitrogen is heated to the first preset temperature range export to lift bed reactor bottom
Portion；
Into lift bed reactor bottom silica flour and nitrogen flow from bottom to top during react generation nitridation
Silicon powder, and tail gas is from reactor head outlet output to bag hose after reacting；
The bag hose is used to carry out gas solid separation processing, and the material of the solid particle in its cavity to tail gas after reaction
When position reaches preset height, the solid particle isolated is exported to lift bed reactor bottom, to continue to participate in reaction, and is divided
The gas separated out is directly vented；
The content that the lift bed reactor is additionally operable to the beta-silicon nitride powder in it stops reaction when reaching preset value, and
It exports and is discharged from reactor bottom after beta-silicon nitride powder cooling in it.
Optionally, the lift bed reactor includes cylinder, gas distribution grid and low head, the cylinder body bottom and lower envelope
Head is connected by gas distribution grid, and gas distributor is provided on the gas distribution grid, gas distribution is provided in the low head
Pipe；The silica flour of silica flour storage tank output enters cylinder body bottom, in the region above gas distribution grid, the high temperature nitrogen of heater output
In region inside into low head, below gas distribution grid, the high temperature nitrogen carries out just by the gas distribution pipe in low head
It after step arrangement, is uniformly distributed using the gas distributor on gas distribution grid, then occurs with the silica flour for entering cylinder body bottom
Reaction generates beta-silicon nitride powder, solid discharge mouth discharge of the beta-silicon nitride powder after cooling through cylinder body bottom.
Optionally, it is provided with temperature measurer on the cylinder, for the temperature of conversion zone in measuring cylinder body, outside the cylinder
Equipped with insulating layer and heating device, the heating device and temperature measurer composed cascade chain control circuit, in conversion zone
Heating device is closed when temperature is more than the peak of the second preset temperature range to stop heating, and low in the temperature of conversion zone
Start heating device when the minimum of the second preset temperature range to begin to warm up, to by the control of the temperature of conversion zone the
In two preset temperature ranges.
Optionally, second preset temperature range is 1100-1350 DEG C；The temperature measurer is using multiple, on cylinder
A temperature measurer is set every one meter, to realize being precisely controlled for bed temperature.
Optionally, the granularity of silica flour is less than 500 mesh, silicone content 99.99-99.999% in silica flour storage tank；It enters to and carries
It is 99.99-100% to rise nitrogen content in the nitrogen of bed reactor bottom；
The temperature range of the low temperature nitrogen is 15-40 DEG C；Low temperature nitrogen is heated to the first default temperature by the heater
Ranging from 1200-1400 DEG C of degree；The preset value of silicon nitride content in lift bed reactor is 99.5%-100%.
Optionally, further include heat exchanger, tail gas after the reaction for being used to export using the outlet of lift bed reactor head
Nitrogen after heating is sent to heater and continues to add by heat to heating without the low temperature nitrogen that heater heats
Heat, and by reaction rear molding pneumatic transmission after cooling toward bag hose.
Optionally, the heat exchanger uses the pipe heat exchanger of vertical installation, wherein reaction rear molding makes tube side, cryogenic nitrogen leave with rage
Make shell side leave with rage.
Optionally, the part nitrogen in the nitrogen after the heating of the heat exchanger output enters it from silica flour tank top
Interior, so that its interior pressure is higher than lift bed reactor internal pressure 50KPa or more, and the nitrogen after remaining heating enters lift bed
Reactor bottom.
Optionally, it is 1 μm that the filter core of the bag hose, which uses metal agglomeration filter core, separation accuracy, separative efficiency 95%,
Operating temperature is 100-500 DEG C；The bag hose uses two, and the using and the reserved are mutually to switch, regular deslagging.
Optionally, the part nitrogen in the nitrogen after the heating of the heat exchanger output enters at the top of bag hose in it,
The solid particle for isolating bag hose as purging nitrogen is purged point by point to lift bed reactor bottom, and after remaining heating
Nitrogen enters lift bed reactor bottom.
Advantageous effect：
The use of high-purity silicon powder is raw material, using promotion in lift bed beta-silicon nitride powder preparation system described in the utility model
Bed reactor carries out nitridation reaction, avoid due to silica flour grain size it is too small caused by not energy fluidizing or fluidized state is bad asks
Topic realizes coming into full contact with for silicon powder particle and nitrogen, and gas-solid phase contact area is big, and reaction rate is fast, yield is big；Lift bed is reacted
Fluid and solid particle heat transfer, mass transfer rate are fast in the reaction bed of device, are convenient for the control of reaction temperature, product quality high.
Description of the drawings
Fig. 1 is the structural schematic diagram for the lift bed beta-silicon nitride powder preparation system that the utility model embodiment provides.
In figure：1- silica flour charge lines；2- silica flour storage tanks；3- silica flours storage tank is to reactor feed line；4- is promoted
Bed reactor；5- gas distribution grids；6- reactor outlets are to heat exchanger pipeline；7- low heads；8- heat exchangers；9- exchanges heat
Device outlet line；10- low temperature nitrogen inlet lines；11- heat exchangers are to heater pipeline；12- heaters；13- heaters
To reactor low head nitrogen pipeline；14- high temperature nitrogens are to silica flour tank line；15- high temperature nitrogens are to bag hose pipeline；
16- bag hoses；17- bag hose gaseous phase outlet pipelines；18- bag hoses are to reactor deslagging pipeline；19- conversion zone scum pipes
Line.
Specific implementation mode
To make those skilled in the art more fully understand the technical solution of the utility model, with reference to the accompanying drawings and examples
The utility model is described in further detail.
The existing technology for preparing silicon nitride there are the problem of include：(1) fixed bed is deposited during preparing beta-silicon nitride powder
The shortcomings of temperature control is difficult, reaction time is long, high energy consumption；(2) fluid bed is prepared during beta-silicon nitride powder to silica flour
It is more demanding, it is difficult to realize industrial applications.
To solve the above-mentioned problems, the utility model provides a kind of improved lift bed beta-silicon nitride powder preparation system, should
The fine silica powder that system is less than 500 mesh using grain size is used as silicon source, is come into full contact with by lift bed realization reaction gas, Guyuan material,
After-treatment system (i.e. bag hose) realizes that the separation of solid particle in tail gas after reaction, the solid particle after separation return to lift bed
Circular response is carried out to improve the preparation efficiency of beta-silicon nitride powder to reduce requirement of the reaction process to silica flour, reduce
Production cost.
It is described in detail below by specific embodiment.
As shown in Figure 1, the utility model embodiment provides a kind of lift bed beta-silicon nitride powder preparation system comprising silica flour
Storage tank 2, lift bed reactor 4, heater 12 (electric heater can be used) and bag hose 16 (sack cleaner can be also referred to as).
Wherein, silica flour for being periodically fed through 4 bottom of lift bed reactor by the silica flour storage tank 2；
The heater 12 is used to after low temperature nitrogen is heated to the first preset temperature range export to lift bed reactor 4
Bottom；
Into 4 bottom of lift bed reactor silica flour and nitrogen flow from bottom to top during react generation nitridation
Silicon powder, and tail gas is from reactor head outlet output to bag hose 16 after reacting；
The bag hose 16 is used to carry out gas solid separation processing, and solid particle in its cavity to tail gas after reaction
When material position reaches preset height (being set according to the actual parameter of bag hose by those skilled in the art), by what is isolated
Solid particle is exported to 4 bottom of lift bed reactor, and to continue to participate in reaction, and (main component is not anti-to the gas isolated
The nitrogen answered) directly emptying；
The content that the lift bed reactor 4 is additionally operable to the beta-silicon nitride powder in it stops reaction when reaching preset value,
And it exports and is discharged from reactor bottom after the beta-silicon nitride powder cooling in it.
Specifically, the lift bed reactor 4 include cylinder, gas distribution grid 5 and low head 7, the cylinder body bottom with
Low head 7 is connected by gas distribution grid 5, and gas distributor is provided on the gas distribution grid 5, is set in the low head 7
It is equipped with gas distribution pipe；The silica flour that silica flour storage tank 2 exports enter cylinder body bottom, the top of gas distribution grid 5 region in, heater 12 is defeated
The high temperature nitrogen (being heated to the nitrogen after the first preset temperature range) gone out enters inside low head 7, below gas distribution grid 5
Region in, the high temperature nitrogen by low head 7 gas distribution pipe carry out tentatively arrange after, using on gas distribution grid 5
Gas distributor be uniformly distributed, then with enter cylinder body bottom silica flour react generate beta-silicon nitride powder, it is after cooling
Solid discharge mouth discharge of the beta-silicon nitride powder through cylinder body bottom.
In addition, being provided with temperature measurer on the cylinder, for the temperature of conversion zone in measuring cylinder body, set outside the cylinder
There are insulating layer and heating device (electric heater unit can be used), the heating device to be returned with temperature measurer composed cascade chain control
Heating device is closed when road for the temperature in conversion zone is more than the peak of the second preset temperature range to stop heating, with
And start heating device when the temperature of conversion zone is less than the minimum of the second preset temperature range to begin to warm up, thus will be anti-
The temperature of section is answered to control in the second preset temperature range.
Wherein, second preset temperature range is 1100-1350 DEG C, i.e., is closed when the temperature of conversion zone is more than 1350 DEG C
Heating device is closed to stop heating, and starts heating device when the temperature of conversion zone is less than 1100 DEG C to begin to warm up.Institute
Temperature measurer is stated using multiple, a temperature measurer is set every one meter on cylinder, to realize being precisely controlled for bed temperature.
In the present embodiment, the granularity of silica flour is less than 500 mesh (i.e. grain size is less than 10 μm) in silica flour storage tank, silicone content is
99.99-99.999%, and the silica flour in silica flour storage tank be periodically sent into time of lift bed reactor can be by those skilled in the art
It is set according to response situation；The nitrogen for entering to lift bed reactor bottom is pure nitrogen gas, and wherein nitrogen content is 99.99-
100%.
The low temperature nitrogen refers to room temperature or nitrogen at room temperature, and temperature range is specially 15-40 DEG C；The heating
It is 1200-1400 DEG C that low temperature nitrogen is heated to the first preset temperature range by device 12；Silicon nitride content in lift bed reactor 4
Preset value be 99.5%-100%.
As shown in Figure 1, the preparation system further includes heat exchanger 8, it is used for defeated using 4 top exit of lift bed reactor
The heat of tail gas heats the low temperature nitrogen heated without heater 12 after the reaction gone out, and by the nitrogen after heating
It is sent to heater 12 to continue to heat, and by reaction rear molding pneumatic transmission after cooling toward bag hose 16.
Specifically, the heat exchanger 8 uses the pipe heat exchanger of vertical installation, wherein reaction rear molding makes tube side, low temperature leave with rage
Nitrogen walks shell side.Specifically, tail gas end socket at the top of the heat exchanger enters tube side after reaction, then from exchanger base end socket from
It opens, and low temperature nitrogen enters shell side from heat exchanger lower part, is then left from heat exchanger top.
More preferably, the part nitrogen in nitrogen after the heating that the heat exchanger 8 exports enters it from 2 top of silica flour storage tank
Interior, so that its interior pressure is higher than lift bed reactor internal pressure 50KPa or more, and the nitrogen after remaining heating enters lift bed
4 bottom of reactor.
In the present embodiment, it is 1 μm that the filter core of the bag hose 16, which uses metal agglomeration filter core, separation accuracy, separative efficiency
It is 95%, operating temperature is 100-500 DEG C；The bag hose 16 uses two, and the using and the reserved are arranged mutually to switch, periodically
Slag.In other words, after the material position of the solid particle in running order bag hose cavity reaches preset height, in its separation
While the solid particle gone out starts output to lift bed reactor bottom, it is switched to another bag hose, i.e., by original place in standby
It is in working condition with the bag hose switching of state, and former in running order bag hose is attached to by reverse blow with removing
The solid particle of cartridge surface to all export the solid particle in cavity to lift bed reactor, then is converted
Working efficiency is improved so as to continuously carry out gas solid separation processing to tail gas after reaction for stand-by state,
More preferably, the part nitrogen in nitrogen after the heating that the heat exchanger 8 exports enters it from 16 top of bag hose
Interior, the solid particle for isolating bag hose 16 as purging nitrogen is purged to 4 bottom of lift bed reactor point by point, and remaining adds
Nitrogen after heat enters 4 bottom of lift bed reactor.
In the present embodiment, three parts can be divided into from the nitrogen after the heating that heat exchanger 8 exports, wherein first part is from silica flour
The top of storage tank 2 enters silica flour storage tank, and second part enters bag hose from 16 top of bag hose, and Part III is from lift bed reactor
4 bottoms enter reactor, can be set according to actual conditions by those skilled in the art as the accounting of each section nitrogen；Or
Person can only be divided into two parts from the nitrogen after the heating that heat exchanger 8 exports, and wherein first part enters from 2 top of silica flour storage tank
Silica flour storage tank, second part enter reactor from 4 bottom of lift bed reactor, can be by this field as the accounting of each section nitrogen
Technical staff sets according to actual conditions；Alternatively, can only be divided into two parts from the nitrogen after the heating that heat exchanger 8 exports,
Wherein first part enters bag hose from 16 top of bag hose, and second part enters reactor from 4 bottom of lift bed reactor, until
It can be set according to actual conditions by those skilled in the art in the accounting of each section nitrogen.Certainly, it is exported from heat exchanger 8
Nitrogen after heating can not also divide and all enter reactor from 4 bottom of lift bed reactor.
The operation principle of preparation system described in the present embodiment is described in detail with reference to Fig. 1：
Granularity is added by silica flour charge line 1 to silicon less than the high-purity silicon powder that 500 mesh, silicone content are more than 99.99%
In powder storage tank 2, the part high temperature nitrogen from heat exchanger 8 is passed through through high temperature nitrogen to silica flour tank line 14 into silica flour storage tank 2
Gas, so that the pressure in silica flour storage tank is higher than 4 internal pressure 50KPa of lift bed reactor or more；By the silica flour in silica flour storage tank 2
By silica flour storage tank to regular 4 bottom of addition lift bed reactor of reactor feed line 3, silica flour and successively through in low head
Gas distributor on gas distribution pipe, gas distribution grid be uniformly distributed after high temperature nitrogen interaction after be dispersed in high temperature nitrogen
To form lift bed (conveying bed), and autoreactor bottom flows up, the conversion zone of lift bed reactor by cylinder outside
Heating device controlled at 1100-1350 DEG C, silica flour and nitrogen, which react, in this temperature range generates silicon nitride powder
Body.Tail gas carrying solid particle comes out reacted device from reactor and is exported in the entrance heat exchanger 8 of heat exchanger pipeline 6 after reaction,
It exchanges heat with the low temperature nitrogen 10 for entering shell side by low temperature nitrogen inlet line 10, tail gas is cooled after reaction, cryogenic nitrogen
Gas is heated.Enter heater 12 through high temperature nitrogen pipeline 11 by the part in the nitrogen of heating, is heated to 1200-
After 1400 DEG C, heated device to reactor low head nitrogen pipeline 13 enters in low head 7, passes through the gas distribution in low head successively
Pipe and gas distribution grid 5 and the gas distributor being installed on it enter conversion zone after being evenly distributed；By in the nitrogen of heating
Another part enters silica flour silica flour storage tank through high temperature nitrogen to silica flour tank line 14；By the remaining nitrogen in the nitrogen of heating
Enter bag hose through high temperature nitrogen to bag hose pipeline 15 and is used as purge gass.Tail gas is through heat exchanger exit pipe after reaction after cooling
Line 9 enters bag hose 16, and the solid particle after reaction in tail gas, which is separated, to be fallen into the cavity of bag hose, and is isolated
Gas (purified reaction end gas) contains minimal amount of dust, and main component is unreacted nitrogen, by bag hose gas phase
Outlet line 17 is directly vented.
After bag hose 16 runs a period of time, the solid particle in cavity increases, when the material position of solid particle in cavity
When reaching certain height, deslagging is switched over to bag hose, the solid particle separated is passed through using high pressure-temperature nitrogen
To reactor deslagging pipeline 18, conversion zone of the purging to lift bed reactor is reacted bag hose with continuing to participate in point by point.
In the cylinder of lift bed reactor, after silica flour reacts a period of time with nitrogen, it is anti-that nitridation occurs for most of silica flour
Silicon nitride should be generated, takes a small amount of sample to be detected from the conversion zone deslagging pipeline 19 being connected with cylinder body bottom, works as silicon nitride
Content when being more than 99% or more, stop reaction, the beta-silicon nitride powder in reactor be discharged after system cooling.
In conclusion the present embodiment, using the silica flour of fine grain as raw material, in lift bed reactor, silica flour is dispersed in successively
In high temperature nitrogen after the gas distribution pipe in low head, the gas distributor on gas distribution grid are uniformly distributed, carried to be formed
Rise bed (conveying bed), during gas-solid phase flows from bottom to top in the cylinder of lift bed reactor, silica flour and nitrogen
It reacts and generates beta-silicon nitride powder；Tail gas enters heat exchanger, the reaction rear molding of high temperature after leaving lift bed reactor after reaction
The nitrogen of gas and low temperature exchanges heat in heat exchanger, and tail gas is cooled after reaction, and low temperature nitrogen is heated；Reaction after cooling
Tail gas enters in bag hose afterwards, wherein the solid particle carried is separated into the cone-shaped cavity of bag hose, needs regular
Solid particle in bag hose is drained into lift bed reactor and continues to participate in reaction；It is anti-from lift bed after reacting a period of time
It answers the sample tap of device to be sampled analysis, when the silicon nitride purity in sample reaches 99.5% or more, stops reaction, will be promoted
Beta-silicon nitride powder discharge in the cylinder of bed reactor, packaging, to complete the preparation work of beta-silicon nitride powder.Therefore, this reality
It applies example and nitridation reaction is carried out using lift bed reactor, reduce requirement of the reaction process to silica flour grain size so that silicon powder particle
Use scope it is wider, it is easy to accomplish industrial applications also improve the preparation efficiency of beta-silicon nitride powder, reduce and be produced into
This.
It is understood that embodiment of above is merely to illustrate that the principles of the present invention and uses exemplary
Embodiment, however the utility model is not limited thereto.For those skilled in the art, this is not being departed from
In the case of the spirit and essence of utility model, various changes and modifications can be made therein, these variations and modifications are also considered as this reality
With novel protection domain.
Claims (10)
1. a kind of lift bed beta-silicon nitride powder preparation system, which is characterized in that including silica flour storage tank, lift bed reactor, heating
Device and bag hose,
Silica flour for being periodically fed through lift bed reactor bottom by the silica flour storage tank；
The heater is used to after low temperature nitrogen is heated to the first preset temperature range export to lift bed reactor bottom；
Into lift bed reactor bottom silica flour and nitrogen flow from bottom to top during react generate silicon nitride powder
Body, and tail gas is from reactor head outlet output to bag hose after reacting；
The bag hose is used to carry out gas solid separation processing to tail gas after reaction, and the material position of the solid particle in its cavity reaches
When to preset height, the solid particle isolated is exported to lift bed reactor bottom, to continue to participate in reaction, and is isolated
Gas be directly vented；
The content that the lift bed reactor is additionally operable to the beta-silicon nitride powder in it stops reaction when reaching preset value, and at it
It exports and is discharged from reactor bottom after interior beta-silicon nitride powder cooling.
2. preparation system according to claim 1, which is characterized in that the lift bed reactor includes cylinder, gas point
Fabric swatch and low head, the cylinder body bottom are connected with low head by gas distribution grid, and gas is provided on the gas distribution grid
Body distributor is provided with gas distribution pipe in the low head；The silica flour of silica flour storage tank output enters cylinder body bottom, on gas distribution grid
In the region of side, the high temperature nitrogen of heater output enters inside low head, in the region below gas distribution grid, the high temperature
Nitrogen uniformly divides after the gas distribution pipe in low head tentatively arrange using the gas distributor on gas distribution grid
Then cloth reacts with the silica flour for entering cylinder body bottom and generates beta-silicon nitride powder, beta-silicon nitride powder after cooling is through cylinder bottom
The solid discharge mouth in portion is discharged.
3. preparation system according to claim 2, which is characterized in that temperature measurer is provided on the cylinder, for measuring
The temperature of conversion zone in cylinder, the cylinder outside are equipped with insulating layer and heating device, and the heating device is constituted with temperature measurer
Heating device is closed in tandem chain control circuit when being more than the peak of the second preset temperature range for the temperature in conversion zone
To stop heating, and start heating device when the temperature of conversion zone is less than the minimum of the second preset temperature range to start
Heating, to control the temperature of conversion zone in the second preset temperature range.
4. preparation system according to claim 3, which is characterized in that second preset temperature range is 1100-1350
℃；A temperature measurer is arranged every one meter on cylinder, to realize the accurate control of bed temperature using multiple in the temperature measurer
System.
5. preparation system according to claim 1, which is characterized in that
The granularity of silica flour is less than 500 mesh, silicone content 99.99-99.999% in silica flour storage tank；Enter to lift bed reactor bottom
Nitrogen content is 99.99-100% in the nitrogen in portion；
The temperature range of the low temperature nitrogen is 15-40 DEG C；Low temperature nitrogen is heated to the first preset temperature model by the heater
Enclose is 1200-1400 DEG C；The preset value of silicon nitride content in lift bed reactor is 99.5%-100%.
6. preparation system according to any one of claims 1-5, which is characterized in that further include heat exchanger, be used for profit
With the heat of tail gas after the reaction of lift bed reactor head outlet output to adding without the low temperature nitrogen that heater heats
Heat treatment, and is sent to heater by the nitrogen after heating and continues to heat, and by reaction rear molding pneumatic transmission after cooling toward bag hose.
7. preparation system according to claim 6, which is characterized in that the heat exchanger uses the pipe type heat transfer of vertical installation
Device, wherein reaction rear molding makes tube side leave with rage, cryogenic nitrogen makes shell side leave with rage.
8. preparation system according to claim 6, which is characterized in that in the nitrogen after the heating of the heat exchanger output
Part nitrogen enters from silica flour tank top in it, so that its interior pressure is higher than lift bed reactor internal pressure 50KPa or more,
And the nitrogen after remaining heating enters lift bed reactor bottom.
9. preparation system according to claim 6, which is characterized in that the filter core of the bag hose is filtered using metal sintering
Core, separation accuracy are 1 μm, and separative efficiency 95%, operating temperature is 100-500 DEG C；The bag hose uses two, and one uses
One it is standby mutually to switch, regular deslagging.
10. preparation system according to claim 9, which is characterized in that in the nitrogen after the heating of the heat exchanger output
Part nitrogen enter in it at the top of the bag hose, purging is extremely point by point for the solid particle isolated bag hose as purging nitrogen
Lift bed reactor bottom, and the nitrogen after remaining heating enters lift bed reactor bottom.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110294465A (en) * | 2019-05-16 | 2019-10-01 | 宁夏秦氏新材料有限公司 | The preparation method of decanter type self- propagating silicon nitride |
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2017
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110294465A (en) * | 2019-05-16 | 2019-10-01 | 宁夏秦氏新材料有限公司 | The preparation method of decanter type self- propagating silicon nitride |
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