CN104925764B - The device of silicon imide serialization generation - Google Patents
The device of silicon imide serialization generation Download PDFInfo
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- CN104925764B CN104925764B CN201510324142.8A CN201510324142A CN104925764B CN 104925764 B CN104925764 B CN 104925764B CN 201510324142 A CN201510324142 A CN 201510324142A CN 104925764 B CN104925764 B CN 104925764B
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Abstract
The present invention provides a kind of device of silicon imide serialization generation, including reactor, for being input into liquefied ammonia, nitrogen and SiCl in the reactor4Input unit and the flash vessel for the product of the reactor to be carried out separation of solid and liquid, it is characterised in that:The reactor includes the spray washing area, reaction zone and the settling zone that set gradually from top to bottom, and the spray washing area, reaction zone and settling zone are integrated.The device of silicon imide serialization generation of the invention, the silicon imide reaction of formation device being integrated by integrated settling zone, SiCl4 distributors, pond separator, reaction zone, spray washing area, double flash evaporation device, has the advantages that flexible operation, high conversion rate, the serialization that product purity is high, material loss is low are generated.
Description
Technical field
The present invention relates to the precursor silicon imide or its polymer/mixture of silicon amine thermal decomposition method generation beta-silicon nitride powder
Serialization generating means, more particularly to a kind of device of silicon imide serialization generation.
Background technology
The beta-silicon nitride powder generated by silicon amine thermal decomposition method is high pure and ultra-fine, al highpHa phases contents, sintering activity high
High-end ceramic material/ceramic matric composite main source (for example prepare ceramic engine/part, large-size ceramic bearing/
Ball).The precursor silicon imide or its polymer/mixture of the beta-silicon nitride powder that research and development is generated by silicon amine thermal decomposition method
New device be active response《New material industry " 12 " development plan》With《New material industry " 12 " major products
Catalogue》To advanced ceramics powder high pure and ultra-fine, and oversize silicon nitride ceramics excellent properties specific requirement.
The synthetic method of the precursor silicon imide of silicon amine thermal decomposition method generation beta-silicon nitride powder has liquid phase method or FCC Off-Gas over Zeolite Catalyst.
The raw material for using is SiCl4(liquid/gas) and NH3(liquid/gas), its general chemistry reaction equation is:
SiCl4+18NH3→1/x[Si(NH)2]x+4NH4Cl.3NH3
Wherein, x is the silication imines degree of polymerization in formula.
The key technology of silicon amine thermal decomposition method generation beta-silicon nitride powder is precursor silicon imide Si (NH)2Generation, silicon is sub-
Amine Si (NH)2Formation efficiency directly affect the output capacity of beta-silicon nitride powder, it is entitled in Application No. 89106804.X
The manufacture method of alpha-silicon nitride powders and the patent of equipment are only disclosed by Japanese UBE companies liquid phase method continuous prodution silicon nitride powder
The thinking at end, in precursor silicon imide Si (NH) of beta-silicon nitride powder2Generating means on also merely disclose a kind of principle
Device, using the device at silicon imide Si (NH)2Generating process in still suffer from that low-temperature operation difficulty is big, solid-liquid washing is separated
The problems such as efficiency and yield are low, thermal decomposition serialization can not be implemented.
The content of the invention
The technical problems to be solved by the invention are:In order to overcome deficiency of the prior art, the present invention to provide a kind of silicon
The device of imines serialization generation, solves existing silicon imide Si (NH)2Decompose generation alpha-silicon nitride powders low-temperature operation difficulty it is big,
Solid-liquid washing separative efficiency and yield is low, thermal decomposition serialization such as can not implement at the technical problem.
The present invention solves its technical problem technical scheme to be taken:A kind of device of silicon imide serialization generation,
Including reactor, for input liquefied ammonia, nitrogen and SiCl in the reactor4Input unit and for by the reactor
Product carry out the flash vessel of separation of solid and liquid, it is characterised in that:The reactor includes that the spray for setting gradually from top to bottom is washed
Area, reaction zone and settling zone are washed, the spray washing area, reaction zone and settling zone are integrated.By spray washing area and reaction
Area integrates can realize that the serialization with spray washing is synthesized, and reach and operate flexible, high conversion rate, product purity
The low purpose of high, material loss.
Further, react generated product major part and enter settling zone, further, since discharging substantial amounts of heat during reaction
Amount, a part of product is by vaporizing ammonia or SiCl4Gas air lift goes out liquid phase into spray washing area, therefore, the flash distillation
Device includes first order flash vessel and second level flash vessel, and the first order flash vessel passes through the first product dump valve and the reaction
Device settling zone is connected, and the product of the settling zone is entered for treatment, and the second level flash vessel passes through the second product dump valve
It is connected with the reactor spray washing area, the product for processing spray washing area.Setting double flash evaporation device, different products/
The mixture of accessory substance can obtain different separation, can obtain the silicon imide product of high-purity or obtain different-grain diameter/specific surface
Long-pending silicon imide product.
Further, the first gas phase dump valve and the first solid phase dump valve, described are additionally provided with the first order flash vessel
One gas phase dump valve is located at the first order flash vessel upper end, for discharging ammonia to aftertreatment systems, first solid phase
Dump valve is located at the first order flash vessel lower end, for discharging solid product, first is additionally provided with the first order flash vessel
Flash vessel gaseous pressure meter and the first seperation film, for controlling the first flash vessel gaseous pressure to reach the purpose of separation of solid and liquid,
In flash process, solid phase finished product can produce tiny particle, the fine particle entrained by purification gas phase, therefore set first and separate
The fine particle that film carries out in first order flash vessel entrained by gas phase is separated with gas phase.
Further, the second gas phase dump valve and second solid phase dump valve, described are additionally provided with the second level flash vessel
Two gas phase dump valves are located at the second level flash vessel upper end, for discharging ammonia to aftertreatment systems, the second solid phase
Dump valve is located at the second level flash vessel lower end, for discharging solid product, second is additionally provided with the second level flash vessel
Flash vessel gaseous pressure meter and the second seperation film, for controlling the second flash vessel gaseous pressure to reach the purpose of separation of solid and liquid,
In flash process, solid phase finished product can produce tiny particle, the fine particle entrained by purification gas phase, therefore set second and separate
The fine particle that film carries out in the flash vessel of the second level entrained by gas phase is separated with gas phase.
Further, the reaction zone is provided with SiCl4Distributor and pond separator, the SiCl4Distributor and pond separator are handed over
For distribution.Liquid phase SiCl4Or gas phase SiCl4SiCl is passed through as carrier using high pure nitrogen4Distributor enters reaction zone with reaction
Vigorous reaction in the liquefied ammonia in area, liquefied ammonia part vaporization in reaction zone there is, take away partial reaction heat.Pond separator is set, will be anti-
Area and settling zone relative separation are answered, reaction yield is effectively improved.
Further, the SiCl4Distributor and pond separator are plumbing installation, the plumbing installation two ends and the reaction
The side wall in area is fixedly connected, the SiCl4The diameter of the plumbing installation of distributor is less than the plumbing installation of the pond separator
Diameter, the SiCl4Perforate is additionally provided with distributor.SiCl4Distributor can implement SiCl using the plumbing installation for being provided with perforate4
Liquid or SiCl4The multiple spot distribution of gas, effectively improves the proposition of by-product ammonium chloride in liquefied ammonia, reduces by-product ammonium chloride and exists
The dissolving of liquefied ammonia, effectively improves the purity of reaction yield and product.Pond separator is set, reaction zone and settling zone are divided relatively
From effectively improving reaction yield.Solid product concentration is high in settling zone, simplifies silicon imide subsequent treatment process, reduces liquefied ammonia
Loss.Used as the splitting equipment for liquid phase being divided into reaction zone and settling zone, its total section will account for reactor and cut pond separator
More than the 50% of face, so the diameter of single plumbing installation is bigger than the plumbing installation diameter of SiCl4 distributor.
Further, the reaction zone is additionally provided with liquid level gauge, and the liquid level gauge is located at the bottom of the reaction zone, and positioned at institute
State SiCl4The top of distributor and pond separator.By the level stability in liquid level gauge maintenance reaction area, reaction is set continuously to enter
OK.
Further, the input unit includes liquefied ammonia input unit, nitrogen inlet device and SiCl4Input unit, respectively
For being input into high-purity liquefied ammonia, high pure nitrogen and high-purity alpha-SiC l4Gas or liquid, the liquefied ammonia input unit include first input end
With the second input, the first input end is connected with the upper end in the spray washing area, and raw materials ammonia is added into spray washing
Area and the SiCl for vaporizing entrainment in ammonia4Gas further reacts, and effectively absorbs the ammonium chloride by-product carried secretly in vaporization ammonia
Thing, realizes the abundant reaction of raw material;Second input is connected with the lower end in the spray washing area, by raw materials ammonia plus
Enter to reaction zone liquid phase, by the level stability in reaction zone liquid level gauge maintenance reaction area, reaction is carried out continuously;The nitrogen
Gas input unit and SiCl4The lower end of the reaction zone is connected to after input unit connection, by the use of high pure nitrogen as SiCl4
The carrier of input.
Further, in order to realize the control to feedstock input rate, the liquefied ammonia input unit, nitrogen inlet device and
SiCl4At least one dump valve and a pressure gauge are equipped with input unit.By the aperture of dump valve come control pressure meter
So as to realize the control to feedstock input rate.
Further, in order to effectively eliminate blocking hidden danger, the spray washing area is provided with packing layer, and described filler layer uses hole
Plate ripple arranged packing.The structure can also promote the further reaction of the SiCl4 gases carried secretly in ammonia, improve reaction and receive
Rate;The ammonium chloride by-product carried secretly in ammonia is effectively absorbed, the purity of reactor tail gas ammonia is improved, is conducive to the follow-up work of ammonia
Effective utilization of sequence.
Specifically, the orifice plate material is PP, ceramics or stainless steel.
Further, the settling zone is additionally provided with level-sensing device.The aperture of the first product dump valve is controlled by level-sensing device, is maintained
The liquid level of settling zone/material position stabilization, reaches the purpose of continuous discharge.
In order to be reused to the liquefied ammonia vaporized in reaction zone, the reactor upper end is provided with the 3rd gas phase dump valve
With reactor gaseous pressure meter.
Specifically, stainless steel or Austenitic Stainless Steel Pressure equipment of the reactor using heat-insulation and heat-preservation.Reaction is needed
Will be under normal temperature or cryogenic conditions, reaction can release substantial amounts of heat, it is necessary to cryogenic refrigeration equipment removes substantial amounts of reaction heat,
The extent of reaction and final reactant purity depend on reaction temperature, so reaction temperature is main technology controlling and process regulation ginseng
Number, thus reactor using heat-insulating heat-preserving material in order to prevent ambient temperature change to reaction zone in reactor come influence, from
And improve the purity of reactant.
The beneficial effects of the invention are as follows:The device of silicon imide serialization of the invention generation, by integrated settling zone,
The silicon imide generation that SiCl4 distributors, pond separator, reaction zone, spray washing area (packing layer), double flash evaporation device are integrated
Reactor, has the advantages that flexible operation, high conversion rate, the serialization that product purity is high, material loss is low are generated.
Brief description of the drawings
The invention will be further described with reference to the accompanying drawings and examples.
Fig. 1 is the optimum embodiment structural representation of the device of silicon imide serialization generation.
Fig. 2 is the front view of SiCl4 distributors and pond separator position in Fig. 1.
Fig. 3 is the top view of SiCl4 distributors and pond separator position in Fig. 1.
In figure:1st, liquefied ammonia input unit, 2, nitrogen inlet device, the 21, the 3rd dump valve, the 22, the 3rd pressure gauge, 3,
SiCl4Input unit, the 31, the 4th dump valve, the 32, the 4th pressure gauge, 4, spray washing area, 5, reaction zone, 6, settling zone, 7,
Primary flash device, 71, first order flash vessel gaseous pressure meter, the 72, first gas phase dump valve, the 73, first solid phase dump valve, 74,
First seperation film, 8, second level flash vessel, 81, second level flash vessel gaseous pressure meter, the 82, second gas phase dump valve, 83, second
Solid phase dump valve, the 84, second seperation film, the 9, first product dump valve, the 10, second product dump valve, 11, first input end,
111st, the first dump valve, 112, first pressure meter, the 12, second input, the 121, second dump valve, 122, second pressure meter, 13,
Liquid level gauge, 14, SiCl4Distributor, 141, perforate, 15, pond separator, 16, level-sensing device, the 17, the 3rd gas phase dump valve, 18, anti-
Answer device gaseous pressure meter.
Specific embodiment
Presently in connection with accompanying drawing, the present invention is described in detail.This figure is simplified schematic diagram, is only illustrated in a schematic way
Basic structure of the invention, therefore it only shows the composition relevant with the present invention.
As Figure 1-3, a kind of device of silicon imide serialization generation of the invention, including input unit, reactor and
Flash vessel, input unit is synthesized for raw material to be input into reactor, and the product after being synthesized enters back into sudden strain of a muscle
Steaming device carries out separation of solid and liquid.
Wherein, input unit includes liquefied ammonia input unit 1, nitrogen inlet device 2 and SiCl4Input unit 3, is respectively used to
It is input into high-purity liquefied ammonia NH3, high pure nitrogen N2With high-purity alpha-SiC l4Gas and/or liquid;Reactor includes setting gradually from top to bottom
Spray washing area 4, reaction zone 5 and settling zone 6, spray washing area 4, reaction zone 5 and settling zone 6 are integrated, can realized
The serialization with spray washing is synthesized, reaches and operates flexible, high conversion rate, the purpose that product purity is high, material loss is low;
Flash vessel includes first order flash vessel 7 and second level flash vessel 8, and first order flash vessel 7 is by the first product dump valve 9 and precipitation
Area 6 is connected, and the product of settling zone 6 is entered for treatment, and second level flash vessel 8 passes through the second product dump valve 10 and spray washing
Area 4 connects, the product for processing spray washing area 4.Double flash evaporation device is set, and the mixture of different product/accessory substances can be obtained
To different separation, the silicon imide product of high-purity or the silicon imide product of acquisition different-grain diameter/specific surface area can be obtained.
Specifically, first turning on the first dump valve 111 and first pressure meter on the first input end 11 of liquefied ammonia input unit 1
112, high-purity liquefied ammonia is input to spray by the first input end 11 of the liquefied ammonia input unit 1 being connected with the upper end of spray washing area 4
Scrubbing section 4 is drenched, meanwhile, the second dump valve 121 and second pressure meter 122 on the input 12 of liquefied ammonia input unit 1 second are opened,
Raw materials ammonia is added to the liquid phase of reaction zone 5 by the second input 12 being connected by the lower end with spray washing area 4;Then, open
The 3rd dump valve 21 and the 3rd pressure gauge 22 on nitrogen inlet device 2 are opened, high pure nitrogen is input into by nitrogen inlet device 2
To reaction zone 5;Finally open SiCl4The 4th dump valve 31 and the 4th pressure gauge 32 on input unit 3, by high-purity alpha-SiC l4First with
Reaction zone 5 is input to again after nitrogen mixing, and is continuously input into high-purity liquefied ammonia, high pure nitrogen and high-purity alpha-SiC l4Liquid and/or gas
Body, three will produce vigorous reaction in reaction zone 5.Dump valve and pressure gauge in above-mentioned are used to realize to feedstock input rate
Control, by the aperture of dump valve come control pressure meter so as to realize the control to feedstock input rate.
Reaction zone 5 is additionally provided with SiCl4Distribution 14 and pond separator 15, SiCl4Distributor 14 and pond separator 15 divide to replace
The plumbing installation of cloth, plumbing installation two ends are fixedly connected with the side wall of reaction zone 5, SiCl4The plumbing installation of distributor 14 it is straight
Footpath is less than the diameter of the plumbing installation of pond separator 15, SiCl4The side wall of the plumbing installation of distributor 14 is provided with perforate 141,
SiCl4The input of distributor 14 and nitrogen inlet device 2 and SiCl4Input unit 3 is connected, and is reacted for reactant.Liquid
Phase SiCl4Or gas phase SiCl4SiCl is passed through as carrier using high pure nitrogen4Distributor 14 enters in reaction zone 5 and reaction zone 5
Liquefied ammonia there is vigorous reaction, the structure can implement SiCl4Liquid or SiCl4The multiple spot distribution of gas, in effectively improving liquefied ammonia
The proposition of by-product ammonium chloride, reduces by-product ammonium chloride in the dissolving of liquefied ammonia, effectively improves the purity of reaction yield and product.
Reaction zone 5 and the relative separation of settling zone 6 are effectively improved solid product in reaction yield, and settling zone 5 dense by pond separator 15
Degree is high, simplifies silicon imide subsequent treatment process, reduces the loss of liquefied ammonia.Nitrogen inlet device 2 and SiCl4The end of input unit 3
It is connected on same input channel, the nitrogen and SiCl being first input into4Mix and then be transported to SiCl again4In distributor 14
Reacted into reaction zone 5 by perforate 141.Pond separator 15 as liquid phase divide into reaction zone 5 and settling zone 6 point
Equipment is cut, its total section will account for more than the 50% of reactor cross section, so the diameter of single plumbing installation is distributed than SiCl4
The plumbing installation diameter of device 14 is big.
In order to realize being carried out continuously for above-mentioned reaction, liquid level gauge 13 is provided with the bottom of reaction zone 5, and positioned at SiCl4Distribution
The top of device 14 and pond separator 15, by the level stability in the maintenance reaction area 5 of liquid level gauge 13, enables reaction to be carried out continuously.
The product of reaction zone 5 is most of to enter settling zone 6 by pond separator 15, and settling zone 6 is provided with level-sensing device 16, passes through
Level-sensing device 16 controls the aperture of the first product dump valve 9, maintains the liquid level/material position stabilization of settling zone 6, reaches the mesh of continuous discharge
's.Product is set to enter first order flash vessel 7 by the first product dump valve 9, by controlling first order flash vessel gaseous pressure meter
71, reach the separation of solid-liquid.
Can discharge substantial amounts of heat during due to reaction makes liquid ammonia vaporization take away partial heat, meanwhile, carried secretly in vaporization ammonia
SiCl4Gas and ammonium chloride by-product enter spray washing area 4.Therefore, spray washing area 4 is provided with packing layer, using orifice plate ripple
Line structured packing, orifice plate material is PP, ceramics or stainless steel, and raw materials ammonia is added and sprayed by first input end 11 by packing layer
Scrubbing section 4, the structure can promote the further reaction of the SiCl4 gases carried secretly in ammonia, improve reaction yield, meanwhile, have
Effect absorbs the ammonium chloride by-product carried secretly in ammonia, improves the purity of reactor tail gas ammonia, is conducive to ammonia subsequent handling
Effectively utilize, and can effectively eliminate raw material input and block hidden danger.Spray washing area 4 can generate a part of product, generation
The liquefied ammonia of product and absorption ammonium chloride by-product passes through collection device and the second product dump valve 10, into second level flash vessel 8,
By controlling second level flash vessel gaseous pressure meter 81, the separation of solid-liquid is reached.
In order to be reused to the liquefied ammonia for vaporizing, reactor upper end is provided with the 3rd gas phase dump valve 17 and reactor gas
Phase pressure meter 18, controls ammonia to enter aftertreatment systems by controlling the aperture of the 3rd gas phase dump valve 17.
Product into needing to carry out separation of solid and liquid after first order flash vessel 7 and second level flash vessel 8, and by the product after separation
Thing sends into subsequent handling, therefore, the upper end of first order flash vessel 7 is provided with the first gas phase dump valve 72 and lower end is provided with the first solid phase row
Go out valve 73, the first gas phase dump valve 72 is used to discharge ammonia to aftertreatment systems, and the first solid phase dump valve 73 is used to discharge admittedly
Phase product, in flash process, solid phase finished product can produce tiny particle, the fine particle entrained by purification gas phase, therefore set
The fine particle that putting the first seperation film 74 is carried out in first order flash vessel 7 entrained by gas phase is separated with gas phase;The second level flashes
The upper end of device 8 is provided with the second gas phase dump valve 82 and lower end is provided with second solid phase dump valve 83, and the second gas phase dump valve 82 is used to arrange
Go out ammonia to aftertreatment systems, second solid phase dump valve 83 is used to discharge solid product, in flash process, solid phase finished product meeting
Tiny particle is produced, the fine particle entrained by purification gas phase, therefore setting the second seperation film 84 carries out second level flash vessel 8
Fine particle entrained by interior gas phase is separated with gas phase.
Because reaction is needed under normal temperature or cryogenic conditions, reaction can release substantial amounts of heat, it is necessary to cryogenic refrigeration equipment
Substantial amounts of reaction heat is removed, the extent of reaction and final reactant purity depend on reaction temperature, so reaction temperature is
Main technology controlling and process regulation parameter, therefore reactor set using the stainless steel or Austenitic Stainless Steel Pressure of heat-insulation and heat-preservation
It is standby, in order to prevent ambient temperature from changing the influence come to reaction zone in reactor, so as to improve the purity of reactant.In addition, the
Primary flash device 7 has difference with second level flash vessel 8 in classification or treating capacity, and most product is in first order flash vessel 7
Separate, least a portion of product is separated in second level flash vessel 8, because reaction condition is different, first order flash vessel 7 and the second level
The product that flash vessel 8 is separated has differences at aspects such as purity, particle diameters.
With above-mentioned according to desirable embodiment of the invention as enlightenment, by above-mentioned description, related staff
Various changes and amendments can be carried out in without departing from the scope of the present invention completely.The technical scope of this invention is not
It is confined to the content on specification, it is necessary to its technical scope is determined according to right.
Claims (13)
1. a kind of device of silicon imide serialization generation, including reactor, for be input into the reactor liquefied ammonia, nitrogen and
SiCl4Input unit and the flash vessel for the product of the reactor to be carried out separation of solid and liquid, it is characterised in that:It is described anti-
Answering device includes spray washing area (4), reaction zone (5) and settling zone (6) for setting gradually from top to bottom, the spray washing area
(4), reaction zone (5) and settling zone (6) integrate, and the flash vessel includes first order flash vessel (7) and second level flash vessel
(8), the first order flash vessel (7) is connected by the first product dump valve (9) with the settling zone (6), and the second level is dodged
Steaming device (8) is connected by the second product dump valve (10) with the spray washing area (4).
2. the device that silicon imide serialization as claimed in claim 1 is generated, it is characterised in that:The first order flash vessel (7)
On be additionally provided with the first gas phase dump valve (72) and the first solid phase dump valve (73), the first gas phase dump valve (72) is positioned at described
First order flash vessel (7) upper end, the first solid phase dump valve (73) is positioned at first order flash vessel (7) lower end, described
The first flash vessel gaseous pressure meter (71) and the first seperation film (74) are additionally provided with primary flash device (7).
3. the device that silicon imide serialization as claimed in claim 1 is generated, it is characterised in that:The second level flash vessel (8)
On be additionally provided with the second gas phase dump valve (82) and second solid phase dump valve (82), the second gas phase dump valve (82) is positioned at described
Second level flash vessel (8) upper end, the second solid phase dump valve (83) is positioned at second level flash vessel (8) lower end, described
The second flash vessel gaseous pressure meter (81) and the second seperation film (84) are additionally provided with two-stage flash device (8).
4. the device that silicon imide serialization as claimed in claim 1 is generated, it is characterised in that:The reaction zone (5) is provided with
SiCl4Distributor (14) and pond separator (15), the SiCl4Distributor (14) and pond separator (15) are alternately distributed.
5. the device that silicon imide serialization as claimed in claim 4 is generated, it is characterised in that:The SiCl4Distributor (14) and
Pond separator (15) is plumbing installation, and the plumbing installation two ends are fixedly connected with the side wall of the reaction zone (5), described
SiCl4The diameter of the plumbing installation of distributor (14) is less than the diameter of the plumbing installation of the pond separator (15), the SiCl4
Perforate (141) is additionally provided with the plumbing installation of distributor (14).
6. the device that silicon imide serialization as claimed in claim 4 is generated, it is characterised in that:The reaction zone (5) is additionally provided with
Liquid level gauge (13), the liquid level gauge (13) positioned at the bottom of the reaction zone (5), and positioned at the SiCl4Distributor (14) and
The top of pond separator (15).
7. the device that silicon imide serialization as claimed in claim 1 is generated, it is characterised in that:The input unit includes liquefied ammonia
Input unit (1), nitrogen inlet device (2) and SiCl4Input unit (3), the liquefied ammonia input unit (1) includes the first input
End (11) and the second input (12), the first input end (11) is connected with the upper end of the spray washing area (4), and described the
Two inputs (12) are connected with the lower end of the spray washing area (4);The nitrogen inlet device (2) and SiCl4Input unit
(3) lower end of the reaction zone (5) is connected to after connecting.
8. the device that silicon imide serialization as claimed in claim 7 is generated, it is characterised in that:The liquefied ammonia input unit (1),
Nitrogen inlet device (2) and SiCl4At least one dump valve and at least one pressure gauge are equipped with input unit (3).
9. the device that silicon imide serialization as claimed in claim 1 is generated, it is characterised in that:The spray washing area (4) sets
There is packing layer, described filler layer uses perforated plate corrugated structured packing.
10. the device that silicon imide serialization as claimed in claim 9 is generated, it is characterised in that:The orifice plate material is PP, pottery
Porcelain or stainless steel.
The device of 11. silicon imide serialization generations as claimed in claim 1, it is characterised in that:The settling zone (6) is additionally provided with
Level-sensing device (16).
The device of 12. silicon imide serialization generations as claimed in claim 1, it is characterised in that:The reactor upper end is provided with
3rd gas phase dump valve (17) and reactor gaseous pressure meter (18).
The device of the 13. silicon imide serialization generation as any one of claim 1-12, it is characterised in that:The reaction
Device uses the stainless steel or Austenitic Stainless Steel Pressure equipment of heat-insulation and heat-preservation.
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