CN106288705B

CN106288705B - Drying blender, processing system and processing method for silicon tetrachloride slag slurry

Info

Publication number: CN106288705B
Application number: CN201610685831.6A
Authority: CN
Inventors: 王建鑫; 熊焰; 吴一兵; 石安平; 章新虎; 乜生良; 郭晓刚; 辛钧启
Original assignee: JIANGXI SAIWEI LDK PHOTOVOLTAIC SILICON TECHNOLOGY Co Ltd
Current assignee: JIANGXI SAIWEI LDK PHOTOVOLTAIC SILICON TECHNOLOGY Co Ltd
Priority date: 2016-08-18
Filing date: 2016-08-18
Publication date: 2019-07-23
Anticipated expiration: 2036-08-18
Also published as: CN106288705A

Abstract

The present invention provides a kind of drying blender of silicon tetrachloride slag slurry in cold hydrogenation process, including shell, agitating shaft, transmission device, shell, which encloses, to be set to form drying chamber, and shell is equipped with inlet port and outlet port；Agitating shaft is lain in a horizontal plane in drying chamber；Agitating shaft includes spindle nose, hollow central siphon, and spindle nose welds together with hollow central siphon, and hollow central siphon is equipped with stirrer paddle, and the first ribbon and the second ribbon are fixed on hollow central siphon by support rod, and are spiraled around hollow central siphon；The hand of spiral on the left and right sides of each comfortable hollow shaft pipe of first ribbon and the second ribbon on the contrary, and the first ribbon it is opposite with the hand of spiral of second ribbon；Under the rotation of agitating shaft, the first ribbon keeps slurry mobile from both sides to centre, and the second ribbon keeps slurry mobile from centre to both sides.The drying blender can make slurry formation circulate, stir more evenly.The present invention also provides the processing system of silicon tetrachloride slag slurry and processing methods.

Description

Drying blender, processing system and processing method for silicon tetrachloride slag slurry

Technical field

The present invention relates to technical field of polysilicon production, and in particular to one kind is for silicon tetrachloride slag slurry in cold hydrogenation process Drying blender, processing system and processing method.

Background technique

Cold hydrogenation is to convert a large amount of silicon tetrachloride as by-product (STC) that generation is reacted in reduction furnace in polycrystalline silicon production to The process system of the raw material trichlorosilane (TCS) of synthesizing polysilicon；The raw material of the process system has silicon powder, STC, hydrogen, HCl Deng reaction product is the mixture, metal chloride and unreacted silicon powder of hydrogen, STC and TCS, the reactional equation being related to Formula has Si+2H₂+3SiCl₄=4SiHCl₃；Si+3HCl=SiHCl₃+H₂.The system by quencher by most of TCS, STC, The separation of the useful material such as hydrogen, (i.e. silicon tetrachloride slag slurry mainly includes silicon to the wet slurry after cold hydrogenation process system chilling Powder, metal chloride, liquid chlorosilane and hydrogen) drain into slurry drying device；Slurry drying device is used to carry out wet slurry Chlorosilane gas and hydrogen are evaporated to recycle by dry heat, and by after drying solid and lye carry out at neutralization Reason.

Existing drying device, have the following problems in use process: slurry is not formed and is circulated, and drying is stirred Journey can generate blind area, and there are the phenomenons that uneven heating is even.Therefore, it is necessary to provide a kind of four chlorinations suitable for cold hydrogenation process The completely new drying system of silicon slurry.

Summary of the invention

In view of this, being fitted the present invention provides a kind of size circulations good fluidity, the drying blender of stirring uniform drying For the dry stirring of silicon tetrachloride slag slurry in cold hydrogenation process, the present invention also provides a kind of processing systems of silicon tetrachloride slag slurry System and processing method.

In a first aspect, the present invention provides a kind of drying blender of silicon tetrachloride slag slurry in cold hydrogenation process, it is described dry Dry blender includes shell, agitating shaft, transmission device, and the shell, which encloses, to be set to form drying chamber, the top and bottom of the shell It is respectively equipped with inlet port and outlet port；The agitating shaft is lain in a horizontal plane in the drying chamber for the drive in the transmission device Slurry in the drying chamber is stirred under dynamic；Wherein, the both ends of the agitating shaft are by bearing seat supports, the stirring Axis includes spindle nose, hollow central siphon, stirrer paddle, support rod, the first ribbon and the second ribbon, the spindle nose and the hollow central siphon Weld together, the hollow central siphon is equipped with stirrer paddle, and first ribbon and the second ribbon are fixed on by support rod On the hollow central siphon, and spiral around the hollow central siphon；First ribbon and each comfortable institute of second ribbon State the hand of spiral on the left and right sides of hollow central siphon on the contrary, and first ribbon and second ribbon hand of spiral phase Instead；Under the rotation of the agitating shaft, first ribbon promotes slurry from the both sides of drying chamber to centre, second spiral shell Band promotes slurry from the centre of the drying chamber to both sides.

Preferably, the side wall of the shell is equipped with end seat, and one end of the agitating shaft passes through end seat and the institute of the shell It states transmission device to be connected, the other end of the agitating shaft is connected with another end seat of shell.

Spiral shell in the application, on the left and right sides of first ribbon and each leisure of second ribbon hollow central siphon It revolves contrary.Specifically, described in the left side of the symmetry axis using the symmetry axis of the vertical direction of the agitating shaft as boundary The hand of spiral of first ribbon be it is left-handed, the hand of spiral of second ribbon is dextrorotation；It is described on the right side of the symmetry axis The hand of spiral of first ribbon is dextrorotation, and the hand of spiral of second ribbon is left-handed.

Preferably, the radial distance of the axis of first ribbon away from the agitating shaft is greater than second ribbon away from described The radial distance of the axis of agitating shaft.That is, first ribbon is greater than the axial projective area of second ribbon；Described first Distance second ribbon of the ribbon away from the dry blender barrel is close.

Preferably, first ribbon is identical as the screw pitch of second ribbon.

Preferably, first ribbon is with the hand of spiral of second ribbon always on the contrary, first ribbon does not have Positioned at the periphery of second ribbon, the two is welded in intersection.

Preferably, the support rod has synchronous Spiral distribution with first ribbon, the second ribbon.

Preferably, the stirrer paddle is around the hollow central siphon screw arrangement.

Preferably, the dry blender further includes collet, and the collet is disposed around the periphery of the shell, and with it is described It forms a heating cavities between shell, filled with conduction oil in the heating cavities, is provided on the collet and heating sky Heat conducting oil inlet, the conduction oil outlet of chamber connection.

Preferably, the heat conducting oil inlet is arranged at the collet of the housing bottom, and the conduction oil outlet setting exists At the collet of the case top.

In the present invention, be equipped on the shell of the dry blender temperature sensor (preferably in the upper left quarter of shell and Right lower quadrant is respectively provided with) for monitoring the temperature of material in shell, the present invention also sets up thermally conductive in drying process for monitoring simultaneously The inlet temperature of oil and the temperature sensor of outlet temperature.

Preferably, the import oil temperature of the conduction oil is stablized 120-125 DEG C (preferably at 125 DEG C).The conduction oil is logical Pump conveying is crossed, to realize the collet internal circulation flow in dry blender.

It is further preferred that the conduction oil can be T66 high temperature heat conductive oil or L-QD330 conduction oil.

It is further preferred that being additionally provided with insulating layer on the shell, the material of the insulating layer is rock wool.

The dry blender that first aspect present invention provides drives the process of the agitating shaft rotation in transmission device In, horizontal positioned agitating shaft is conducive to stir up and down by material, then in oppositely oriented the first ribbon, the second ribbon Under cooperation, material is formd in drying chamber and is circulated, and stirring material thoroughly without dead angle, is uniformly mixed dried material, Wall not easy to stick, it is also prevented from caking.Even in addition, the material for thering is part to agglomerate, the mistake that stirrer paddle can also be mobile in slurry Material in journey by part agglomeration is smashed, and keeps slurry more tiny.It is to be dried after circulation terminates, soliqueous material is Pass through the discharge port under the agitation of one ribbon to be discharged.The dry blender can make silicon tetrachloride slag slurry in cold hydrogenation process Formation circulates, stirs uniform drying, so as to further technique application.

Preferably, shaft end seal component, institute are additionally provided between the both ends spindle nose of the agitating shaft and the end seat of the shell Shaft end seal component is stated for seal the gap between the agitating shaft and the shell.

Preferably, the shaft end seal component includes spiral sleeve, end seat bushing, seal cartridge, close in seal cartridge Seal labyrinth chamber, packing seal chamber, filler, liquid silicon tetrachloride sealing, nitrogen-sealed and gland, wherein the helical axis It is set on agitating shaft, the spiral sleeve is equipped with external screw thread at the cooperation with the end seat；The end seat bushing, sealing Bushing is sequentially fixed at the inner sidewall of the end seat, on lateral wall, and is set on the spiral sleeve, the end seat lining Set, the seal cartridge with the spiral sleeve clearance fit；The end seat bushing be equipped with on the spiral sleeve The oppositely oriented internal screw thread of external screw thread, is sequentially formed with from inside to outside between the seal cartridge and the mating surface of the spiral sleeve Labyrinth seal chamber, packing seal chamber；The packing seal is intracavitary to be equipped with filler, and the gland is socketed in the spiral sleeve On, and be located by connecting with the outer end of the seal cartridge to compress filler；Institute's labyrinth seal is intracavitary to be equipped at intervals with multiple sealings Piece is additionally provided with the groove for assembling the diaphragm seal on the spiral sleeve；It is successively offered respectively on the seal cartridge Silicon tetrachloride (STC) entrance, nitrogen inlet, for respectively to intracavitary conveying STC, Xiang Suoshu packing seal chamber of the labyrinth seal It is passed through nitrogen inside to be respectively formed STC sealing, nitrogen-sealed.

Preferably, the spiral sleeve and the agitating shaft transition fit, the spiral sleeve are fixed by screws in institute It states on agitating shaft.

Preferably, the external screw thread on the internal screw thread and the spiral sleeve on the end seat bushing has between 0.2-0.6mm Gap.

It is further preferred that the external screw thread is trapezoidal bull external screw thread；The internal screw thread is trapezoidal multiple-internal screw thread.

Preferably, the diaphragm seal is vertically arranged in that the labyrinth seal is intracavitary, and the diaphragm seal does not touch the labyrinth At the top of the cavity of seal chamber, the diaphragm seal is in the intracavitary formation throttle clearance of the labyrinth seal and expansion cavity.

It is further preferred that the diaphragm seal is ring packing piece, the ring packing piece is fixed on by snap ring In the groove.

Preferably, it is polytetrafluoroethylene (PTFE) that the filler, which is material, and the shape of the filler is rectangular.

Preferably, in the side close to the gland, the packing seal is intracavitary to be additionally provided with packing press ring.

Preferably, first gas distribution set and second gas distribution set, the sealing lining are welded on the seal cartridge Set covers upper first aperture with first gas distribution by the silicon tetrachloride entrance and communicates, and the seal cartridge passes through institute Nitrogen inlet is stated to communicate with upper second aperture of second gas distribution set.

Preferably, the first gas distribution set and second gas distribution put on and are respectively welded first flange seat and second Flange seat；The first flange seat is used to take over by first flange and connect with silicon tetrachloride (STC) pipeline, the second flange Seat is connect for being taken over by second flange with nitrogen pipeline.

It is further preferred that the first gas distribution set, second gas distribution set are to be welded on the seal cartridge circle The sleeve of circumferential direction.

It is highly preferred that the first flange adapter tube is also connected with a nitrogen pipeline, so that silicon tetrachloride is passed through low pressure nitrogen It is intracavitary that gas (0.4MPa) is delivered to the labyrinth seal.

In the application, the silicon tetrachloride is sealed into labyrinth seal is intracavitary and conveys tetrachloro using low-pressure nitrogen (0.4MPa) SiClx.The silicon tetrachloride of gas leakage after can preventing drying in this way, sealing can be by being located at the dry stirring Silicon tetrachloride storage tank supply outside device.Silicon tetrachloride is in conveying (in silicon tetrachloride storage tank, silicon tetrachloride pipeline and the first method In orchid adapter tube) it is liquid, when it reaches seal cartridge (labyrinth seal chamber), because temperature increases, (dry blender has conduction oil Heating) and become gaseous state.The nitrogen-sealed be respectively to the intracavitary input low-pressure nitrogen (0.4MPa) of packing seal, the purpose is to Silicon tetrachloride sealing is prevented to be not thorough.

As previously mentioned, the both ends of the spindle nose of the agitating shaft are connected with the end seat of the shell respectively, part spindle nose is pierced by The shell.Wherein be cased with spiral sleeve on agitating shaft, with end seat cooperation at, with the end seat bushing that is fixed in end seat it Between be clearance fit, the screw thread on spiral sleeve and the end seat bushing is on the contrary, under the rotation of the agitating shaft, and material is in phase Eddy generation friction between anti-spiral generates pressure to overcome leakage, constitutes first of sealing of the dry blender.Remote On direction from the shell end seat, be pierced by the part agitating shaft of the shell also have labyrinth seal, silicon tetrachloride sealing, Packing seal and nitrogen-sealed.Spiral sleeve forms band with the seal cartridge being fixed in end seat in the region for being fixed with diaphragm seal The labyrinth seal chamber of labyrinth gap, can be effectively by slurry, and the air seal generated in dry whipping process is here, resistance Only particle travels further into packing seal chamber, forms second sealing, while the STC sealing being connected with labyrinth seal chamber, defeated The STC sent, which enters cavity, can be further reduced the leakage of gas by pressure, form three seals, packing seal, and The nitrogen-sealed communicated therewith sequentially forms the four, the 5th sealings, when micro dust enters packing seal chamber with gas, benefit They can be pushed back in dry blender with the sealing blocking of filler, nitrogen purging.

Preferably, a gas vent is additionally provided at the top of the shell.The gas vent is for connecting a filter, institute Filter is stated for being filtered, purifying to the gas that the slurry generates in whipping process.

In the present invention, it is additionally provided with a pressure sensor in the gas outlet of the dry blender, it is dry for monitoring Pressure during dry.

Preferably, when the shell body temperature of the dry blender differs within 5 DEG C with the outlet temperature of the conduction oil (such as can be 0.2 DEG C, 0.5 DEG C, 1 DEG C, 2 DEG C, 3 DEG C or 4 DEG C), and the pressure in the dry blender 0.1~ When within the scope of 0.5bar, an arid cycle is completed.

It is further preferred that the shell body temperature differs 1-3 with heat transfer oil outlet temperature when completing an arid cycle ℃.More preferably differ within 1 DEG C.

When completing an arid cycle, the pressure in the dry blender be can be within the scope of 0.1-0.3bar, It can be within the scope of 0.2-0.4bar, be also possible within the scope of 0.2-0.45bar.It is further preferred that the drying is stirred The pressure in device is mixed within the scope of 0.2~0.3bar.

Quantization is segmented to the index in drying process in the present invention, the adjusting to arid cycle may be implemented, can save The energy, lowering apparatus loss.In one embodiment of the invention, the arid cycle is 4-7 hours, such as can be 4,5,5.5 or 6 Hour.

The shaft end seal component of dry blender described herein, sealing effect is good, reduces letting out for dry blender It divulges a secret danger, can effectively extend the service life of the dry blender.Even if in dried material containing inflammable, corrosivity etc. at Part, it is also not susceptible to safety accident, pollution will not be generated to environment.

To sum up, the drying blender that first aspect present invention provides can be such that dried material formation circulates, dry There is no stirring blind area, stirrings to be heated more uniform for whipping process；Its sealing effect for drying blender shaft end seal component is good, does The disclosure risk of material is small in dry blender.

Second aspect, the present invention provides the silicon tetrachloride slag slurry processing systems in a kind of cold hydrogenation process, including drying Blender, filter, chlorosilane recycling can and washing packet.

Wherein, the dry blender is provided by first aspect present invention, and the dry blender is used for cold hydrogenation The silicon tetrachloride slag slurry that technique generates is heated, is stirred, and chlorosilane gas and slurry solids are isolated.

The filter takes the chlorosilane gas out of for being filtered to the chlorosilane gas isolated Adsorbing powder dust on the filter bag of the filter, obtain chlorosilane clean gas, the filter is also used to being adsorbed on filter Dust on bag is blown, and falls into the dust in the dry blender.

Further, the filter includes tank body, and end socket is equipped with above the tank body, is equipped with card in the tank body, The inner cavity of tank body is divided into the toilet and filter chamber being distributed up and down by the card, and cage bone is equipped on the card, described Filter bag is cased on cage bone；The side wall of the toilet is equipped with the outlet of net gas and nitrogen inlet, the bottom of the tank body offer gas Body dust import, the filter chamber are communicated with the fuel gas and dust import；Wherein, the filter further includes pulse of nitrogen blowing Device, and the pulse control instrument of the control pulse of nitrogen blowing device, the pulse of nitrogen blowing device include nitrogen into Pipe, solenoid valve, multiple injection tubes and nozzle；The pulse of nitrogen blowing device is equipped with multiple solenoid valves, each electromagnetism Valve is used to control the opening and closing of nitrogen in an injection tube, and the injection tube is connected to the nitrogen by the cylinder of the solenoid valve Inlet pipe, the injection tube are equipped with multiple nozzles, and the mouthpiece of the nozzle is located at the surface of the filter pocket openings, the electromagnetism Valve is electrically connected with the pulse control instrument.

The fuel gas and dust import of the filter is connected with the gas vent of above-mentioned dry blender.Dusty gas is from described Agitated dryer enters the filter；Dust under blowing off when the filter blowing filter bag also falls to the dry stirring In device.

Preferably, the pulse of nitrogen blowing device further includes the nitrogen heater being mounted on outside the tank body, described Nitrogen inlet connects the nitrogen heater by the nitrogen inlet.

It is further preferred that the nitrogen preset temperature is first heated to by the nitrogen heater after just be blown it is clear Ash.The preset temperature is preferably 90-130 DEG C.

Preferably, flange is equipped between the end socket and the tank body.

Preferably, the solenoid valve is located on the end socket, the cylinder of one end of the injection tube and the solenoid valve it Between pass through the flanged joint.

Preferably, the filter bag is polyfluortetraethylefilm film coated filter bag.

Preferably, the aperture of the filter bag is 800-1200 mesh.

Preferably, the net gas outlet is located on the not ipsilateral side wall in the toilet with the nitrogen inlet.It is described net Gas outlet, the nitrogen inlet are respectively positioned on the top of the cage bone.

Preferably, the distance of bottom of the nitrogen inlet away from the tank body is greater than the bottom of the net gas outlet away from tank body Distance, i.e., the position of the described nitrogen mouth is higher than the net gas outlet.

Preferably, the periphery of the tank body is also enclosed equipped with collet, and the collet has heating cavities, the heating of the collet Filled with conduction oil in cavity, for the filter to be maintained certain temperature.

The heat conducting oil inlet being connected to the heating cavities, conduction oil outlet are provided on the collet.Preferably, described Collet at end socket is equipped with conduction oil outlet, and the collet of the filter tank base is equipped with heat conductive oil inlet.

Preferably, the toilet and the filter chamber are mounted on pressure sensor, are used for monitoring pressure in real time.

Preferably, also there is dump mouth on the end socket.

Preferably, also there is water content detection mouth and gas composition detection mouth on the end socket.

Silicon tetrachloride slag slurry isolated chlorosilane gas and slurry solids after dry stirring, wherein chlorosilane gas It can further be filtered by the filter to remove the dust of deentrainment, and by the purging of pulse of nitrogen blowing device by dust It returns again into dry blender, is neutralized in washing packet together with the slurry solids, makes solid-state waste residue It is effectively addressed；The recycling and filtered clean gas can be condensed, enters back into cold hydrogenation process and re-uses.It is described The structure of filter is simple, and operation pressure drop is up to 800Pa, and filter effect is good, also preferable to the purging effect of filter bag, filter bag Infrequently, replacement in about 180 days is primary for replacement.

The chlorosilane recycling can for recycling the chlorosilane clean gas, and condenses the steam into chlorosilane liquid produced, institute Chlorosilane liquid produced is stated to be recycled for being delivered in cold hydrogenation process.The chlorosilane recycling can and the filter Net gas outlet connection.

The washing packet is for carrying out the slurry solids with the dust for falling into dry blender by lye Neutralization reaction is hydrolyzed, and the solidliquid mixture after the neutralization reaction is discharged.

It preferably, further include transhipment tank, the transhipment tank is connect with the discharge port of the dry blender, the transhipment tank The slurry solids is received, and employs nitrogen as and the slurry solids is transported in washing packet for carrier.

Preferably, the top of the chlorosilane recycling can has a condenser, and the condenser is clean by the chlorosilane Gas is condensed into chlorosilane liquid produced, and condensed chlorosilane liquid produced is flow in recycling can；The bottom of the chlorosilane recycling can is also With a delivery pump, the delivery pump is for the chlorosilane liquid produced to be delivered in the quencher in cold hydrogenation process.

The silicon tetrachloride slag slurry processing system in cold hydrogenation process that second aspect of the present invention provides, can be by silicon tetrachloride Slurry is adequately circulated, and efficiently separates to obtain chlorosilane gas and slurry solids, chlorosilane gas can by into The filtering of one step is returned again to dust into dry blender by impulse blowing with removing the dust of deentrainment, together with the slag Slurry solids is neutralized in washing packet together, and solid-state waste residue is made to be effectively addressed；And filtered clean gas Can be condensed recycling, enter back into cold hydrogenation process and re-use.The processing system can effectively solve silicon tetrachloride slag The emission problem of slurry, energy saving, protection environment.

The third aspect, the present invention provides the silicon tetrachloride slag slurry processing method in a kind of cold hydrogenation process, including it is following Step:

(1) silicon tetrachloride slag slurry for generating cold hydrogenation process imports dry blender, right in the dry blender The silicon tetrachloride slag slurry is heated, is stirred, and chlorosilane gas and slurry solids are isolated, wherein the dry stirring Device is provided by first aspect present invention；

(2) chlorosilane gas enters in the filter of the dry whip topping, and the filter is to the chlorine Silane gas is filtered, and the dust that the chlorosilane gas is taken out of is attracted on the filter bag of the filter, obtains chlorine silicon Alkane clean gas, under the blowing of the filter, the dust being adsorbed on filter bag is fallen into the dry blender；

(3) the chlorosilane clean gas enters the chlorosilane recycling being connected with the filter, and is condensed into Chlorosilane liquid produced, the chlorosilane liquid produced are recycled for being delivered in cold hydrogenation process；

(4) the slurry solids is expelled in washing packet with the dust for falling into dry blender, is washed described It washs in packet, the slurry solids and the dust and lye are hydrolyzed neutralization reaction, and by the solid-liquid after the neutralization reaction Mixture discharge.

Preferably, the slurry solids and the dust for falling into dry blender are first expelled in a transhipment tank, institute It states transhipment tank to connect with the discharge port of the dry blender, the transhipment tank employs nitrogen as the slurry solid as carrier Object and the dust are transported in washing packet.

The silicon tetrachloride slag slurry processing method in cold hydrogenation process that third aspect present invention provides, process flow is simple, Low energy consumption, high to the rate of recovery of useful material.

Beneficial effects of the present invention include the following aspects:

1, the agitating shaft being horizontally arranged in dry blender is equipped with the first oppositely oriented ribbon of specific structure, second Ribbon can be such that silicon tetrachloride slag slurry formation circulates, not viscous wall, not agglomerate, stir uniform drying；

2, the sealing effect of the shaft end seal component of dry blender is good, it is possible to reduce the disclosure risk of dry blender, The service life of the dry blender can effectively be extended；

3, the structure for the filter being connected with dry blender is simple, separates after dry stirring to silicon tetrachloride slag slurry The filter effect of the chlorosilane gas arrived is preferable, purging effect of the pulse of nitrogen blowing device in the filter to filter bag Preferably, the replacement of filter bag is infrequently；

4, heat-conducting oil heating is all made of in the collet of dry blender and filter, heating is without dead zone, flow velocity height, heat transfer effect Fruit is high, highly-safe；

5, the processing system of the silicon tetrachloride slag slurry can effectively solve the emission problem of silicon tetrachloride slag slurry, save energy Source, protection environment；The processing method of the silicon tetrachloride slag slurry, process flow is simple, and low energy consumption, to the rate of recovery of useful material It is high.

Detailed description of the invention

Fig. 1 is the structural schematic diagram of dry blender in the embodiment of the present invention；

Fig. 2 is the structural schematic diagram of agitating shaft in the embodiment of the present invention；

Fig. 3 is distribution schematic diagram of first ribbon on agitating shaft in the embodiment of the present invention；

Fig. 4 is distribution schematic diagram of second ribbon on agitating shaft in the embodiment of the present invention；

Fig. 5 is the schematic diagram for the race way that agitating shaft is formed in stirring in the embodiment of the present invention；

Fig. 6 is the structural schematic diagram of the running part of dry blender in Fig. 1, bearing block part, axis shaft end seal part；

Fig. 7 is the enlarged structure schematic diagram of shaft end seal assembly in Fig. 1；

Fig. 8 is the schematic diagram of spiral sleeve in Fig. 7；

Fig. 9 is the schematic diagram of Fig. 7 middle-end seat pad set；

Figure 10 is the enlarged diagram of the labyrinth seal chamber in Fig. 7 on seal cartridge；

Figure 11 is the schematic diagram of seal cartridge in Fig. 7；

Figure 12 is the structural schematic diagram of filter in the embodiment of the present invention；

Figure 13 is that the solenoid valve of filter in the embodiment of the present invention is not powered on closed state (A) and energization open state (B) Schematic diagram；

Figure 14 is the top view of the end socket of filter in the embodiment of the present invention；

Figure 15 is the structural schematic diagram of silicon tetrachloride slag slurry processing system in the embodiment of the present invention.

Specific embodiment

Below in conjunction with the attached drawing in embodiment of the present invention, the technical solution in embodiment of the present invention is carried out clear Chu is fully described by.

Also referring to Fig. 1-Figure 11, silicon tetrachloride slag in a kind of cold hydrogenation process provided for the preferred embodiment of the present invention The structural schematic diagram of the drying blender 100 of slurry.

The dry blender 100 includes shell 1, agitating shaft 2, transmission device 3 (label is not shown in Fig. 1), the shell Body 1, which encloses, to be set to form drying chamber, and the top and bottom of the shell 1 are respectively equipped with feed inlet 11 and discharge port 12, preferably, institute State the center that discharge port 12 is located at 1 bottom of shell.The agitating shaft 2 is lain in a horizontal plane in the drying chamber for described The slurry in the drying chamber is stirred under the driving of transmission device 3.The left and right ends of the agitating shaft 2 are by bearing block 5 supports, the bearing block 5 are the rotation and support that agitating shaft both ends are realized by bearing and support.

As shown in Fig. 2, the agitating shaft 2 includes spindle nose 21, hollow central siphon 22, stirrer paddle 23, support rod 24, the first spiral shell Band 25 and the second ribbon 26, the spindle nose 21 weld together with the hollow central siphon 22, and the hollow central siphon 22 is equipped with and stirs It mixes blade 23, first ribbon 25 and the second ribbon 26 to be fixed on the hollow central siphon 22 by support rod 24, and spirals Around the hollow central siphon 22；Hand of spiral phase of first ribbon 25 on the left and right sides of the hollow central siphon 22 Instead, with the hand of spiral of second ribbon 26 on the left and right sides of the hollow central siphon 22 on the contrary, and first ribbon 25 is opposite with the hand of spiral of second ribbon 26；Under the rotation of the agitating shaft 2, first ribbon 25 by slurry from The both sides of drying chamber are promoted to centre, and second ribbon 26 promotes slurry from the centre of the drying chamber to both sides.

First ribbon 25 and the spiral on the left and right sides of each leisure of second ribbon 26 hollow central siphon 22 It is contrary.Specifically, as shown in Figure 3 and Figure 4, it is with the symmetry axis (dotted line in Fig. 2) of the vertical direction of the agitating shaft 2 Boundary, in the left side of the symmetry axis, the hand of spiral of first ribbon 25 is left-handed, the hand of spiral of second ribbon 26 For dextrorotation；On the right side of the symmetry axis, the hand of spiral of first ribbon 25 is dextrorotation, the spiral of second ribbon 26 Direction is left-handed.

In the application, the first oppositely oriented ribbon 25 of hollow 22 left and right sides of central siphon, equal 2 center of rotation direction agitating shaft will Slurry is promoted from two sides of drying chamber to centre simultaneously；The second oppositely oriented ribbon 26 of hollow 22 the right and left of central siphon, will starch Material is promoted from the centre of the drying chamber to both sides；Due to the spiral of the first ribbon 25 and the second ribbon 26 on hollow central siphon 22 Contrary, the first ribbon 25 and the second ribbon 26 push the direction of slurry movement different, are sufficiently mixed convenient for feed liquid.

As shown in Figure 3 and Figure 4, the radial distance D1 of axis of first ribbon 25 away from the agitating shaft 2 is greater than described The radial distance D2 of axis of second ribbon 26 away from the agitating shaft 2.That is, diameter (the axis projection face of first ribbon 25 Product) it is greater than the diameter (axial projective area) of second ribbon 26；First ribbon 25 is away from 100, the dry blender The distance of wall second ribbon 26 is close.It is understood that the first ribbon 25, the second ribbon 26 are stirred with the drying The barrel of device 100 has a certain distance.

In present embodiment, the screw pitch L1 of first ribbon 25 is identical as the screw pitch L2 of second ribbon 26.

In the application, first ribbon 25 is identical as the screw pitch of second ribbon 26, oppositely oriented, the axial direction of the two Projected area is unequal.First ribbon 25 surround the hollow central siphon 22, but described first with second ribbon 26 Ribbon 25 is not located at the periphery of second ribbon 26, and the two is welded in intersection.

First ribbon 25, the second ribbon 26 are to bend to helix shape by band-like steel band.The embodiment of the present invention In, the stirrer paddle 23 is welded on the hollow central siphon 22.First ribbon 25, the second ribbon 26 are all to pass through branch Strut 24 is connected on hollow central siphon 22.

In present embodiment, the support rod 24 is with first ribbon 25, the second ribbon 26 with synchronous spiral point Cloth.Better supporting role can be played to first ribbon 25, the second ribbon 26 in this way.

In an embodiment of the present invention, the stirrer paddle 23 is around hollow 22 screw arrangement of central siphon.

The dry blender 100 further includes collet 4, and the collet 4 is disposed around the periphery of the shell 1, and with it is described It forms a heating cavities between shell 1, filled with conduction oil in the heating cavities, is provided with and the heating on the collet 4 Heat conducting oil inlet 13, the conduction oil outlet 14 of cavity connection.

Preferably, the bottom of the shell 1 is arranged in heat conducting oil inlet 13, the conduction oil outlet 14 is arranged described The top of shell 1.

In the application, wet slurry-silicon tetrachloride slag slurry under the stirring of dry blender 100 with the conduction oil in collet 4 It carries out heat exchange indirectly and the chlorosilane gas in wet slurry is evaporated, without short circuit, dead zone, flow velocity is high for heating, heat transfer It is high-efficient, chlorosilane gas and slurry solids can be isolated.It is described to lead for use steam is as heat medium The heat transfer efficiency of hot oil is high, and the safety of conduction oil is good, and inertia is low, will not react with chlorosilane, and the temperature of conduction oil It is constant, convenient for manipulation.

In embodiments of the present invention, the conduction oil can be T66 high temperature heat conductive oil or L-QD330 conduction oil.

In an embodiment of the present invention, insulating layer (not shown) is additionally provided with outside the shell 1.The collet 4 can be reduced The volatilization of interior conduction oil, the material of the insulating layer can be rock wool.Dot in Fig. 1 on shell 1 is to be welded on cylinder The small cylinder of small cylinder, these protrusions is for the ease of insulating layer to be coated on shell.

Wherein, the side wall of the shell is equipped with end seat 16, and one end of the spindle nose 21 is passing through the end seat on the shell 1 It is connected after 16 with the transmission device 3.

In an embodiment of the present invention, the transmission device 3 is mounted on the side wall of the shell 1.The transmission device 3 It is connected with the agitating shaft 2, sends power to agitating shaft 2, drives the agitating shaft 2 to rotate, and then in drying chamber Material be stirred, it is sufficiently dry convenient for carrying out the material in drying chamber.

Further, the transmission device 3 includes motor 31, shaft coupling 32, retarder 33, minor sprocket 34, big sprocket wheel 35. The motor 31 connect transmission with the agitating shaft 2 by shaft coupling 32, retarder 33, minor sprocket 34, big sprocket wheel 35.

The carrying out practically of the drying blender 100 is as follows, and motor 31 rotates after energization, drives to deceleration by shaft coupling 32 Device 33, retarder 33 realize the reduction of revolving speed, and retarder 33 and minor sprocket (drive sprocket) 34 pass through axis connection.Minor sprocket 34 is logical It crosses chain (not shown) and drives to big sprocket wheel (by movable sprocket) 35 (rotating ratio of large and small sprocket wheel is 1:3), big sprocket wheel 35 passes through again The connection of round end flat key drives agitating shaft 2 to rotate.

When being ready for stirring, conduction oil is passed through in the collet 4 of dry blender 100, dry blender 100 starts Wet slurry is added in drying chamber, in agitating shaft 2 by heating after temperature reaches the temperature of technique requirement by feed inlet 11 Under rotation, wet slurry constantly recycles in drying chamber, is passed into the conduction oil indirect heating of collet 4, at the same in ribbon and It is sufficiently mixed under the stirring of stirrer paddle 23, the solid residue after drying is expelled to washing packet from the discharge port 12 among drying machine It handles, the gas evaporated in wet slurry can enter filter from the gas vent on dry blender 100, and it is single to reach recycling Member is recovered.

In an embodiment of the present invention, the dry blender 100 further includes rack 6, the shell 1 and the transmission Device 3 is installed in the rack 6.The rack 6 is to fix and support shell 1, motor 31, shaft coupling 32, retarder 33 equal components, the rack 6 can be by the steel structure platform of channel steel, angle steel welding.

In the application, during transmission device 3 drives the agitating shaft 2 to rotate, horizontal positioned agitating shaft 2 is advantageous It is stirred above and below carrying out material, then under the cooperation of oppositely oriented the first ribbon 25, the second ribbon 26, material is in drying chamber It inside foring and circulates, stirring material thoroughly without dead angle, is uniformly mixed dried material, and wall not easy to stick is also prevented from caking, Arid cycle (charging, dry stirring, discharging) is also greatly shortened simultaneously.Even in addition, the material for thering is part to agglomerate, agitating paddle Leaf 23 can also smash the material that part is agglomerated during slurry is mobile, keep slurry more tiny.It is to be dried to follow After ring, soliqueous material is discharged under the agitation of the first ribbon 25 by the discharge port 12.

In addition, slurry can be formed by 4 race ways (such as Fig. 5) using agitating shaft shown in Fig. 2 in the application, because This, dry blender provided by the invention is more full and uniform to the stirring of slurry, stirring efficiency is higher.It is dry that slurry can also be saved The discharge time afterwards.

In an embodiment of the present invention, between the both ends spindle nose 21 of the agitating shaft 2 and the end seat 16 of the shell 1 also Equipped with shaft end seal component 200, the shaft end seal component 200 is used for seal between the agitating shaft 2 and the shell 1 Gap.It is understood that the stirring shaft drive 3, bearing block 5 and shaft end seal component 200 are in the agitating shaft 2 On be disjunct unitary part (such as Fig. 6, Fig. 6 are the enlarged drawings in Fig. 1 on the left of shell).The shell of dry blender 100 in Fig. 1 Have bearing block 5 and shaft end seal component 200 at left and right sides of body, section view only do not carried out to the left side, it is seen that be appearance； Section view is carried out to the right, it can be seen that internal structure.

Please also refer to Fig. 7-Figure 11, the shaft end seal component 200 include spiral sleeve 211, with the end seat 16 according to End seat bushing 212, the seal cartridge 213 of secondary connection, labyrinth chamber sealing 214 in seal cartridge 213, are filled out packing seal chamber 215 Material 216, gland 217, liquid silicon tetrachloride (STC) sealing and nitrogen-sealed.

The spiral sleeve 211 is set on the spindle nose of the agitating shaft 2.Preferably, the spiral sleeve 211 with it is described 2 transition fit of agitating shaft, the spiral sleeve 211 are fixed by screws on the agitating shaft 2.The helixseal set 211 External screw thread 230 is equipped at the cooperation with the end seat 16.It is additionally provided on the spiral sleeve 211 for assembling diaphragm seal 218 Groove 219 (referring to Fig. 8).

The end seat bushing axle sleeve 212 is successively fixedly mounted on the inner sidewall of the end seat 16, outside with seal cartridge 213 On wall, the end seat bushing 212, the seal cartridge 213 are set on the spiral sleeve 211.

The end seat bushing 212 and 211 clearance fit of spiral sleeve, the end seat bushing 212 be equipped with it is described The oppositely oriented internal screw thread 231 of external screw thread 230 on spiral sleeve (referring to Fig. 9).Preferably, the external screw thread 230 is ladder Shape bull external screw thread；The internal screw thread 231 is trapezoidal multiple-internal screw thread.Pressure head caused by the multiple thread of trapezoidal cross-section compared with Height, and the pressure head that trapezoidal multiple thread generates is smaller with gap variation.

The external screw thread 230 on internal screw thread 231 and the spiral sleeve 211 on the end seat bushing 212 has 0.2-0.6mm Gap.Under the rotation of the agitating shaft 2, the material between spiral sleeve 211 and end seat bushing 212 is between opposite spiral Eddy generation friction generates pressure head to overcome the leakage rate of material.The revolving speed of agitating shaft is higher, and amount of leakage is fewer.

The seal cartridge 213 and 211 clearance fit of spiral sleeve, the seal cartridge 213 and the helical axis It is sequentially formed with labyrinth seal chamber 214, packing seal chamber 215 from inside to outside between the mating surface of set 211.

It is understood that the formation of labyrinth seal chamber 214, packing seal chamber 215, is since seal cartridge 213 is in phase It answers position to be equipped with groove and is formed this 2 cavitys when it is arranged with 211 phase of spiral sleeve.

Referring to Figure 10, it is equipped at intervals with multiple diaphragm seals 218 in institute's labyrinth seal chamber 214, on the spiral sleeve 211 also Equipped with the groove 219 for assembling the diaphragm seal 218.

It is further preferred that the diaphragm seal 218 is ring packing piece, the ring packing piece 218 passes through snap ring 220 are fixed in the groove 219 of the spiral sleeve 211.

In the application, multiple diaphragm seals 218 are equipped at intervals in labyrinth seal chamber 214.Diaphragm seal 218 can be it is vertical or with Vertical direction is arranged at an angle in labyrinth seal chamber 214.Preferably, the diaphragm seal 218 is vertically arranged in institute It states in labyrinth seal chamber 214, the diaphragm seal 218 does not touch at the top of the cavity of the labyrinth seal chamber 214.In this way, described close Mounting 218 forms throttle clearance and expansion cavity in the labyrinth seal chamber 214.Wherein, the throttle clearance refers to sealing Gap between at the top of the cavity of piece 218 and the labyrinth seal chamber 214, the expansion cavity refer to that sealed medium exists Gap after throttle clearance, between reached adjacent seals piece 218.Sealed medium (a small amount of slurry and slurry agitation mistake The gas generated in journey) labyrinth seal chamber may be reached by the gap between spiral sleeve and end seat bushing.They will be passed through Labyrinth seal chamber will be having many bends or curves general like labyrinth by route shown in arrow in Figure 10.Sealed medium is passing through It generates throttle effect when gap in tortuous labyrinth seal chamber 214 and achievees the purpose that prevent leakage.

The packing seal chamber 215 is provided with filler 216, and the gland 217 is socketed in the spiral sleeve 211 On, and be located by connecting with the outer end of the seal cartridge 213 to compress filler 216.

In an embodiment of the present invention, it is polytetrafluoroethylene (PTFE) that the filler 216, which is material, the shape of the filler 216 It is rectangular.

In an embodiment of the present invention, in the side close to the gland 217, in the packing seal chamber 215 It is additionally provided with packing press ring 221.

Silicon tetrachloride (STC) entrance, nitrogen inlet are successively offered on the seal cartridge 213 respectively, is used for described It is close to be respectively formed STC sealing, nitrogen to be passed through nitrogen in conveying STC, Xiang Suoshu packing seal chamber 215 in labyrinth seal chamber 214 Envelope.

1 (filler in packing cavity 215, diaphragm seal and card in labyrinth seal chamber 214 are not shown on figure referring to Figure 1 Ring), first gas distribution set 222 and second gas distribution set 223, the first gas are welded on the seal cartridge 213 Distribution set 222 is equipped with the first aperture 224, and the second gas distribution set 223 is equipped with the second aperture 225.The seal cartridge 213 It is communicated by the liquid silicon tetrachloride entrance with the first aperture 224 on first gas distribution set 222, the sealing lining Set 213 is communicated by the nitrogen inlet with the second aperture 225 on second gas distribution set 223.Preferably, sealing Bushing 213 be equipped with 4-6 equally distributed nitrogen inlets, silicon tetrachloride entrance with respectively with first gas distribution set 222 and Second gas distribution 223 phases of set communicate.The number of the first aperture 224 on first gas distribution set 222 can be 1 or more It is a, preferably 4-6.The number of the second aperture 225 on second gas distribution set 223 is also possible to one or more, preferably 4-6.

First flange seat 226 and the are respectively welded on first gas distribution set 222 and second gas distribution set 223 Two flange seats 227；The first flange seat 226 is used to connect by first flange adapter tube 228 with silicon tetrachloride (STC) pipeline, The second flange seat 227 by second flange adapter tube 229 with nitrogen pipeline for being connect.By taking nitrogen-sealed as an example, sealing is used Nitrogen pass sequentially through nitrogen pipeline, second flange adapter tube (nitrogen flange connecting pipe) 229 to the second gas on second flange seat 227 Body distribution set 223, then entered in packing seal chamber 215 by the nitrogen inlet.Sealing nitrogen enters cavity and relies on pressure, can To prevent sealed medium (gas generated during slurry agitation) leakage.

In an embodiment of the present invention, the first gas distribution set 222, second gas distribution set 223 are to be welded on The sleeve of 213 circumferencial direction of seal cartridge.

The first flange adapter tube 228 is also connected with a nitrogen pipeline, so that silicon tetrachloride is passed through low-pressure nitrogen (0.4MPa) is delivered in the labyrinth seal chamber 214.

In the application, the silicon tetrachloride is sealed into labyrinth seal chamber 214 using low-pressure nitrogen (preferably 0.4MPa) convey silicon tetrachloride.Gas leakage after can preventing drying in this way.The silicon tetrachloride of sealing can be by position Silicon tetrachloride storage tank supply outside the dry blender 100.Silicon tetrachloride is in conveying (in silicon tetrachloride storage tank, four In chlorination silicone and first flange adapter tube) it is liquid, when it reaches seal cartridge (labyrinth seal chamber), because temperature increases (dry blender have heat-conducting oil heating) and become gaseous state.It, can also will here in another embodiment of the application Silicon tetrachloride sealing in labyrinth seal chamber 214 changes nitrogen-sealed into.

The nitrogen-sealed is respectively to input low-pressure nitrogen (preferably 0.4MPa) into packing seal chamber 215, purpose It is that the silicon tetrachloride sealing is prevented to be not thorough.

The both ends spindle nose 21 of agitating shaft 2 described herein is connected with the end seat 16 of the shell 1 respectively, part spindle nose 21 It is pierced by the shell.Wherein, be cased with spiral sleeve 211 on agitating shaft 2, with 16 cooperation of end seat at, and be fixed on end seat 16 On end seat bushing 212 between be clearance fit, spiral sleeve 211 is with the screw thread on the end seat bushing 212 on the contrary, described Under the rotation of agitating shaft, slurry eddy generation friction between spiral sleeve 211 and end seat bushing 212 generates pressure to overcome Leakage rate constitutes first of sealing of the dry blender 100.On the direction far from the shell end seat 16, it is pierced by institute Stating on the part agitating shaft of shell 1 also has labyrinth seal 214, silicon tetrachloride sealing, packing seal 215 and nitrogen-sealed.Spiral shell Spin axis set 211 is formed with the seal cartridge 213 being fixed in end seat 16 with labyrinth gap in the region for being fixed with diaphragm seal 218 Labyrinth seal chamber 214, can be effectively by slurry, and the air seal generated in dry whipping process is here, prevent particle The STC sealing for traveling further into packing seal chamber 215, forming second sealing, while being connected with labyrinth seal chamber 214, Enter the leakage that cavity can be further reduced gas by pressure-feed STC, forms three seals, packing seal chamber 215 and interior filler 216, and the nitrogen-sealed being connected to packing seal chamber 215 sequentially forms the four, the 5th sealings, when When micro dust and gas enter packing seal chamber 215, they can be pushed back to using the sealing blocking of filler, nitrogen purging In dry blender 100.

The shaft end seal component 200 of dry blender 100 described herein, sealing effect are good, it is possible to reduce dry The disclosure risk of blender 100 can effectively extend the service life of the dry blender 100.Even if containing in dried material There are the compositions such as inflammable, corrosivity, be also not susceptible to safety accident, pollution will not be generated to environment.

The top of the shell 1 is additionally provided with a gas vent 15.The gas vent 15 is used to connect a filter 700, The filter 700 can be used for being filtered the gas that silicon tetrachloride slag slurry generates in whipping process, purify, so as to mistake Gas after filter is further utilized.

In the present invention, it is additionally provided with a pressure sensor at the gas vent 15 of the dry blender, for monitoring Pressure in drying process.

Preferably, when the shell body temperature of the dry blender differs within 5 DEG C with the outlet temperature of the conduction oil, And the pressure in the dry blender within the scope of 0.1~0.5bar when, complete an arid cycle.

It is further preferred that the shell body temperature when the dry blender differs 1 with the outlet temperature of the conduction oil Within DEG C, and when the pressure in the dry blender is within the scope of 0.2~0.3bar, an arid cycle is completed.The present invention In in drying process index segment quantization, the adjusting to arid cycle may be implemented, can save the energy, lowering apparatus damage Consumption.

Also referring to Figure 12-Figure 14, for a kind of structural representation for filter 700 that the preferred embodiment of the present invention provides Figure.The filter 700 includes tank body 71, and end socket 72 is equipped with above the tank body 71, and card 73 is equipped in the tank body, described The inner cavity of tank body 71 is divided into two parts up and down by card 73, and top is toilet, and lower part is filter chamber, is pacified on the card 73 Equipped with cage bone 74, filter bag 75 is cased on the cage bone 74；The side wall of the toilet is equipped with net gas outlet 711 and nitrogen inlet 712, the bottom of the tank body 71 offers fuel gas and dust import 713, the filter chamber and 713 phase of fuel gas and dust import It is logical；Wherein, the filter 700 further includes pulse of nitrogen blowing device, and the arteries and veins of the control pulse of nitrogen blowing device Controller is rushed, the pulse of nitrogen blowing device includes nitrogen inlet 80, solenoid valve 81, multiple injection tubes 82 and nozzle 83；Institute It states pulse of nitrogen blowing device and multiple solenoid valves 81 is installed, each solenoid valve 81 is for controlling nitrogen in an injection tube 82 The opening and closing of gas, the injection tube 82 are connected to the nitrogen inlet 80, the injection tube 82 by the cylinder of the solenoid valve 81 Multiple nozzles 83 are equipped with, the mouthpiece of the nozzle 83 is located at the surface of the filter bag 75 opening, the solenoid valve 81 and institute State pulse control instrument electrical connection.

The fuel gas and dust import 713 is connected with the gas vent 15 of above-mentioned dry blender 100.Dusty gas is from described Agitated dryer 100 enters the filter 700；Dust under the filter 700 is blown off when being blown filter bag also falls to institute It states in dry blender 100.

In an embodiment of the present invention, the pulse of nitrogen blowing device further includes the nitrogen being mounted on outside the tank body 71 Hot-air heater, the nitrogen inlet 80 connect the nitrogen heater by the nitrogen inlet 712.

It is understood that the pulse of nitrogen blowing device is connected with compressed nitrogen gas source.The nitrogen of blowing is by institute The offer of compressed nitrogen gas source is provided.

It is further preferred that the nitrogen set temperature is first heated to by the nitrogen heater after just be blown it is clear Ash.The preset temperature is preferably 90-130 DEG C.It can prevent in this way during blowing that metal chloride, chlorosilane etc. is cold It coagulates, in order to avoid influence the effect of blowing filter bag.

Flange 70 is equipped between the end socket 72 and the tank body 71.In the embodiment of the application, the end socket 72 further preferably ball crown type, the middle parts of the tank body 71 are cylindrical shape.

The solenoid valve 81 is located on the end socket, between one end of the injection tube 82 and the cylinder of the solenoid valve 81 It is connected by the flange 76.

Referring to Figure 13, the enlarged drawing for the spool 813 that the rightmost side in A, B is solenoid valve is schemed.Solenoid valve 81 described herein Also there is a cylinder 811, the cylinder 811 of the solenoid valve 81 welds together with the end socket 72 on filter, and shape is integral, The cylinder 811 of solenoid valve 81 is connected on the flange 70；The valve head of solenoid valve 81 is fixed by screws on cylinder.Work as electromagnetism When valve 81 is not powered on, the flexible sheet 812 of the spool 813 of solenoid valve 81 and nitrogen inlet 80 be in closed state, nitrogen into For nitrogen in pipe 80 only in the outside of 81 cylinder of solenoid valve, nitrogen does not enter the injection tube 82 being connected with the cylinder of solenoid valve 81 Interior (A in Figure 13)；When solenoid valve 81, which is powered, to be opened, the flexible sheet 812 of solenoid valve 81 moves up under magneticaction, nitrogen Gas just enters in the injection tube 82 being connected to solenoid valve 81 (B in Figure 13).

In the application, the cylinder of the solenoid valve 81 is connected with the nitrogen inlet 80.Preferably, the solenoid valve 81 Cylinder be staggered for two rows, the cylinder of preferably 2 solenoid valves 81 is directly connected with the nitrogen inlet duct 80, remaining The cylinder of solenoid valve 81 realizes the connection with nitrogen inlet 80 indirectly by the cylinder of this 2 solenoid valves 81 again.

In an embodiment of the present invention, the injection tube 82, the number of solenoid valve 81 are 4, in an injection tube 82 Multiple nozzles 83 can be extended, face filter bag 75 is open the mouthpiece of the nozzle 83 vertically downward.

In the application, it is evenly distributed with hole on the card 73, cage bone 74 is installed in hole, by screw by the cage bone 74 are fixed on card 73, and filter bag 75 is cased on cage bone 74.

In an embodiment of the present invention, the filter bag 75 is polyfluortetraethylefilm film coated filter bag.The friction system of polytetrafluoroethylene (PTFE) Number is low, chemical stability is good, can high temperature resistant, surface it is smooth, greatly reduce filter pressure, the table of polyfluortetraethylefilm film coated filter bag Face is easily cleared up, and makes to filter substantially continuous operation.In addition, the intensity of polytetrafluoroethylene (PTFE) is higher, last a long time.

In an embodiment of the present invention, the aperture of the filter bag 75 is 800-1200 mesh.

In an embodiment of the present invention, the net gas outlet 711 is located at the toilet not with the nitrogen inlet 712 On ipsilateral side wall.The net gas outlet 711, the nitrogen inlet 712 are respectively positioned on the top of the cage bone 74.

In an embodiment of the present invention, the distance of bottom of the nitrogen inlet 712 away from the tank body 71 is greater than described net Gas exports the distance of 711 bottoms away from tank body 71, i.e., the position of the described nitrogen inlet 712 is higher than the net gas outlet 711.

The periphery of the tank body 71 is also enclosed equipped with collet 76, and the collet 76 has heating cavities, and the collet 76 adds Filled with conduction oil in hot cavity, for the filter 700 to be maintained certain temperature (100 DEG C or so, 100-120 DEG C), with It prevents the material (metal chloride, chlorosilane etc.) into filter 700 from condensing out, generates crystal, block filter, shadow Ring filter effect.The heat transfer efficiency of the conduction oil is high, and the safety of conduction oil is good, and inertia is low, and the temperature of conduction oil It is constant, convenient for manipulation.

The heat conducting oil inlet 714 being connected to the heating cavities, conduction oil outlet 715 are provided on the collet 76.It is excellent Selection of land, the collet of 71 bottom of tank body are equipped with heat conductive oil inlet 714, and the collet at the end socket 72 goes out equipped with conduction oil Mouth 715.

The toilet and the filter chamber are mounted on pressure sensor, are used for monitoring pressure in real time.

In the application, the pulse control instrument is the impulse generator for controlling solenoid valve 81 and acting.Pulse control instrument electricity consumption Cable is connected on PLC (programmable logic controller (PLC)).The solenoid valve 81 preferably passes through cable and the pulse control instrument phase Connection.

The fuel gas and dust import 713 is connected with a dry blender.Dusty gas enters institute from the agitated dryer State filter；Dust under blowing off when the filter blowing filter bag is also fallen in the dry blender.

Filtration condition: after in the tank body 71 that dust-laden chlorosilane gas enters filter 700 through fuel gas and dust import 713, A part under the action of primary settling and self gravity, is settled down to and is connected with the fuel gas and dust import 713 compared with coarse granule dirt In the drying blender connect.After thinner dust enters filter chamber, in filter bag two sides under the action of pressure difference, by Blang diffusion and The combined effects such as sieving are attracted on 75 surface of filter bag, and purified gas passes through filter bag 75 and enters toilet, via net gas 711 discharge of outlet, separative efficiency can achieve >=99.9%.

Jetting deashing state: with the continuous progress of filtering operating condition, the dust that product is attached on 75 surface of filter bag will constantly increase Add, the operation pressure drop of the filter 700 increases, and filtration resistance is continuously increased, and to work normally the filter 700, needs Dust stratification on filter bag 75 is periodically removed.When the pressure drop of the toilet of the equipment and filter chamber reaches setting value, close Net gas outlet regulates and controls the pulse control instrument to start pulse of nitrogen blowing device, and solenoid valve 81 is opened, and nitrogen passes through the nitrogen Hot-air heater is heated to preset temperature (such as 100 DEG C or so), enters the mistake from nitrogen inlet 80 via nitrogen inlet 712 In the tank body 71 of filter 700, hot nitrogen sprays under the control of each solenoid valve 81 from the nozzle 83 that corresponding each injection tube 82 connects It is blown to filter bag 75, all dust for being attached to product on 75 surface of filter bag are fallen, and are fallen back again via the fuel gas and dust import 713 Into dry blender, filter bag 75 can be put back into.The dust for falling back dry blender can be stirred together with dry The slurry solids obtained after device stirring is discharged together.

Referring to Figure 14, also there is dump mouth 721 on the end socket 72, the dump mouth 721 is connected with safety Valve.When net gas outlet 711 blocks or causes gas that can not be discharged because of other, pass through fuel gas and dust import 713 and the filtering The connected dry blender of device 700 constantly evaporates gaseous state chlorosilane, will lead to 700 superpressure of filter, when described After 400 superpressure of filter, by 721 pressure release of dump mouth, the gas in the filter 700 is drained into dump System, so that pressure is in a certain range in system.

Also there is water content detection mouth 722 and gas composition detection mouth 723 on the end socket 72.More perfect filter Function keeps cold hydrogenation process system more environmentally friendly, safe.

Silicon tetrachloride slag slurry chlorosilane gas and slurry solids isolated after dry stirring, the filter 700 can carry out chlorosilane gas further filtering to remove the dust of deentrainment, and blowing by pulse of nitrogen blowing device It sweeps and returns again to dust into dry blender 100, be neutralized in washing packet together with the slurry solids, Solid-state waste residue is set to be effectively addressed；And filtered clean gas can be condensed recycling, enter back into weight in cold hydrogenation process It is new to utilize.The structure of the filter 700 is simple, and operation pressure drop is up to 800Pa, and filter effect is good, imitates to the purging of filter bag Fruit is also preferable, filter bag is replaced infrequently, and replacement in about 180 days is primary.

The present invention also provides the silicon tetrachloride slag slurry processing systems in a kind of cold hydrogenation process, and structural schematic diagram is as schemed Shown in 15, the silicon tetrachloride slag slurry processing system includes dry blender 100, filter 700,400 He of chlorosilane recycling can Washing packet 600.

Wherein, the dry blender 100 is used to generate cold hydrogenation process as shown in the above-mentioned any figure of Fig. 1-Figure 11 Silicon tetrachloride slag slurry heated, stirred, isolate chlorosilane gas and slurry solids.

The filter 700 is as shown in the above-mentioned any figure of Figure 12-Figure 14, the fuel gas and dust import 713 of the filter 700 It is connect with the gas vent 15 of the dry blender 100, the filter 700 has pulse of nitrogen blowing device；The mistake Filter 700 is used for the adsorbing powder dust that the chlorosilane gas isolated is filtered, and the chlorosilane gas is taken out of On the filter bag 75 of the filter 700, chlorosilane clean gas is obtained, the pulse of nitrogen blowing device is used for being adsorbed on Dust on filter bag 75 is blown, and falls into the dust in the dry blender 100.

The chlorosilane recycling can 400 is connect with the net gas of the filter 700 outlet 711, the chlorosilane recycling can 400 for recycling the chlorosilane clean gas, and condenses the steam into chlorosilane liquid produced, and the chlorosilane liquid produced is for being delivered to It is recycled in cold hydrogenation process.

The washing packet 600 is used for through lye to the slurry solids and the powder for falling into dry blender 100 Neutralization reaction is hydrolyzed in dirt, and the solidliquid mixture after the neutralization reaction is discharged.

Wherein, silicon tetrachloride slag slurry processing system further includes transhipment tank 500, the transhipment tank 500 and the dry stirring The discharge port 12 of device 100 connects, and the transhipment tank 500 receives the slurry solids, and employing nitrogen as will be described for carrier Slurry solids is transported in washing packet 600.It is understood that the transhipment tank is equipped with feed inlet and discharge gate, it is described The discharge port for transporting tank is connected with the outlet of the washing packet, the discharging of the feed inlet and the dry blender of the transhipment tank Mouth is connected.

In an embodiment of the present invention, the top of the chlorosilane recycling can 400 has a condenser, the condenser The chlorosilane clean gas is condensed into chlorosilane liquid produced, condensed chlorosilane liquid produced is flow in recycling can；The chlorine silicon The bottom of alkane recycling can also has a delivery pump, and the delivery pump is for the chlorosilane liquid produced to be delivered in cold hydrogenation process Quencher in.

In the application, the hydrolysis neutralization reaction carried out in the washing packet 600, is the common knowledge of this field, in institute Stating the chemical reaction occurred in washing packet 600 has:

SiCl₄+2H₂O→SiO₂+4HCl；

SiHCl₃+3H₂O→SiO₂+H₂O+3HCl+H₂；

NaOH+SiO₂+H₂O→Na₂SiO₃·nH₂O。

The silicon tetrachloride slag slurry processing system in cold hydrogenation process that second aspect of the present invention provides, can be by silicon tetrachloride Slurry is adequately circulated, and efficiently separates to obtain chlorosilane gas and slurry solids, chlorosilane gas can by into The filtering of one step is returned again to dust into dry blender by impulse blowing with removing the dust of deentrainment, together with the slag Slurry solids is neutralized in washing packet together, and solid-state waste residue is made to be effectively addressed；And filtered clean gas Can be condensed recycling, enter back into cold hydrogenation process and re-use.The processing system effectively solves silicon tetrachloride slag slurry Emission problem has saved the energy, has accomplished environmental protection.

The present invention also provides the silicon tetrachloride slag slurry processing methods in cold hydrogenation process, comprising the following steps:

(1) silicon tetrachloride slag slurry that cold hydrogenation process generates is imported into dry stirring described in the above-mentioned any figure of Fig. 1-Figure 11 In device 100, the silicon tetrachloride slag slurry is heated in the dry blender 100, is stirred, chlorosilane gas is isolated With slurry solids；

(2) chlorosilane gas enters the dry blender 100 by the gas vent 15 of the dry blender In the filter 700 at top, the filter 700 as shown in the above-mentioned any figure of Figure 12-Figure 14, but not limited to this；The filtering Device 700 is filtered the chlorosilane gas, and the dust that the chlorosilane gas is taken out of is attracted to the filter 700 On filter bag 75, chlorosilane clean gas is obtained, under the blowing of the pulse of nitrogen blowing device of the filter 700, is adsorbed on The dust on filter bag 75 is fallen into the dry blender 100；

(3) the chlorosilane clean gas, which enters, goes out the 711 mouthfuls of chlorosilanes connecting recycling with the net gas of the filter 700 Tank 400, and chlorosilane liquid produced is condensed into chlorosilane recycling can 400, the chlorosilane liquid produced is for being delivered to cold hydrogenation It is recycled in technique；

(4) the slurry solids is expelled in washing packet 600 with the dust for falling into dry blender 100, In washing packet 600, the slurry solids and the dust and lye are hydrolyzed neutralization reaction, and by the neutralization reaction Solidliquid mixture discharge afterwards.

In one embodiment of the invention, the arid cycle is 5-7 hours.Specifically: the silicon tetrachloride slag slurry (wet pulp Material) enter the pressure about 0.5bar after dry blender, heat-conducting oil heating in the collet through dry blender 100, operative liquid Slurry gradually flashes to chlorosilane gas, dry at this time pressure rise in blender 100 to 1~2bar (preferably at 1~ 1.5bar), the time of pressure buildup phase is 1~2 hour；The gas evaporated enters filter 700, passes through filter top Filter bag after, via filter net gas outlet 711 enter chlorosilane recycling cans 400, chlorosilane recycling can 400 pass through its pressure Regulating valve makes entire silicon tetrachloride slag slurry processing system (refer mainly to dry blender 100, filter 700, chlorosilane recycling can 400) pressure is maintained at 2bar hereinafter, passing through the safety valve pressure release of drying machine filter top if pressure-regulating valve failure. After liquid slurry all flashes to gas, the pressure in the dry blender drops to 0.7bar or so (0.6-0.7bar), It is slowly declined to 0.2~0.3bar from 0.7bar again, the time in this stage is 4~5 hours, and so far, the dry blender is complete At an arid cycle.

In the embodiment of the present invention, the slurry solids and the dust for falling into dry blender are first expelled to transhipment tank In 500, the transhipment tank 500 is connect with the discharge port of the dry blender 100, the transhipment tank 500 employ nitrogen as The slurry solids and the dust are transported in washing packet 600 by carrier.

The top of the chlorosilane recycling can has a condenser, and the condenser condenses the chlorosilane clean gas At chlorosilane liquid produced, condensed chlorosilane liquid produced is flow in recycling can；The bottom of the chlorosilane recycling can also has one defeated Pump is sent, the delivery pump is for the chlorosilane liquid produced to be delivered in the quencher in cold hydrogenation process.

The above is a preferred embodiment of the present invention, and but it cannot be understood as to the invention patent range Limitation.It should be pointed out that for those skilled in the art, without departing from the principle of the present invention, also Several improvements and modifications can be made, these modifications and embellishments are also considered to be within the scope of the present invention.

Claims

1. the drying blender of silicon tetrachloride slag slurry in a kind of cold hydrogenation process, which is characterized in that the dry blender includes Shell, agitating shaft, transmission device, the shell, which encloses, to be set to form drying chamber, and charging is respectively equipped at the top and bottom of the shell Mouth and discharge port；The agitating shaft is lain in a horizontal plane in the drying chamber for doing under the driving of the transmission device to described Dry intracavitary slurry is stirred；Wherein, the both ends of the agitating shaft are by bearing seat supports, the agitating shaft include spindle nose, Hollow central siphon, stirrer paddle, support rod, the first ribbon and the second ribbon, the spindle nose weld together with the hollow central siphon, The hollow central siphon is equipped with stirrer paddle, and first ribbon and the second ribbon are fixed on the hollow central siphon by support rod On, and spiral around the hollow central siphon；First ribbon and each leisure of second ribbon hollow central siphon The hand of spiral on the left and right sides on the contrary, and first ribbon it is opposite with the hand of spiral of second ribbon；It is stirred described Under the rotation for mixing axis, first ribbon by slurry from the both sides of drying chamber to centre promote, second ribbon by slurry from The centre of the drying chamber is promoted to both sides；

Shaft end seal component, the shaft end seal group are additionally provided between the both ends spindle nose of the agitating shaft and the end seat of the shell Part includes spiral sleeve, end seat bushing, seal cartridge, sealing labyrinth chamber, packing seal chamber, filler in seal cartridge, liquid Silicon tetrachloride sealing, nitrogen-sealed and gland, wherein the spiral sleeve is set on agitating shaft, the spiral sleeve External screw thread is equipped at the cooperation with the end seat；The end seat bushing, seal cartridge are sequentially fixed at the inside of the end seat On wall, lateral wall, and be set on the spiral sleeve, the end seat bushing, the seal cartridge with the helical axis Cover clearance fit；The end seat bushing is equipped with the internal screw thread oppositely oriented with the external screw thread on the spiral sleeve, described close It is sequentially formed with labyrinth seal chamber, packing seal chamber from inside to outside between envelope bushing and the mating surface of the spiral sleeve；It is described to fill out Material seal chamber is provided with filler, and the gland is socketed on the spiral sleeve, and fixed with the outer end of the seal cartridge Position connection is to compress filler；Institute's labyrinth seal is intracavitary to be equipped at intervals with multiple diaphragm seals, is additionally provided with and is used on the spiral sleeve Assemble the groove of the diaphragm seal；Silicon tetrachloride entrance, nitrogen inlet are successively offered on the seal cartridge respectively, for dividing Not to the intracavitary conveying silicon tetrachloride of the labyrinth seal, Xiang Suoshu packing seal is intracavitary is passed through nitrogen to be respectively formed silicon tetrachloride Sealing, nitrogen-sealed.

2. dry blender as described in claim 1, which is characterized in that first ribbon and each leisure of the second ribbon The hand of spiral on the left and right sides of the hollow central siphon on the contrary, specifically:

Using the symmetry axis of the vertical direction of the hollow central siphon as boundary, in the left side of the symmetry axis, the spiral shell of first ribbon Revolve direction be it is left-handed, the hand of spiral of second ribbon is dextrorotation；On the right side of the symmetry axis, the spiral shell of first ribbon Rotation direction is dextrorotation, and the hand of spiral of second ribbon is left-handed.

3. dry blender as described in claim 1, which is characterized in that the axis of first ribbon away from the agitating shaft Radial distance is greater than the radial distance of the axis of second ribbon away from the agitating shaft；First ribbon and second spiral shell The screw pitch of band is identical.

4. dry blender as described in claim 1, which is characterized in that the dry blender further includes collet, the folder Set is disposed around the periphery of the shell, and a heating cavities are formed between the shell, filled with thermally conductive in the heating cavities Oil is provided with the heat conducting oil inlet being connected to the heating cavities, conduction oil outlet on the collet.

5. dry blender as described in claim 1, which is characterized in that the diaphragm seal is vertically arranged in the labyrinth seal Intracavitary, the diaphragm seal does not touch at the top of the cavity of the labyrinth seal chamber, and the diaphragm seal is in the intracavitary shape of the labyrinth seal At throttle clearance and expansion cavity.

6. dry blender as described in claim 1, which is characterized in that internal screw thread and the spiral on the end seat bushing External screw thread on axle sleeve has the gap of 0.2-0.6mm；The external screw thread is trapezoidal bull external screw thread；The internal screw thread is trapezoidal more Head internal screw thread.

7. the silicon tetrachloride slag slurry processing system in a kind of cold hydrogenation process, which is characterized in that any including such as claim 1-6 Drying blender described in, filter, chlorosilane recycling can and washing packet.

8. processing system as claimed in claim 7, which is characterized in that the filter includes tank body, is set above the tank body There is end socket, is equipped with card in the tank body, the inner cavity of tank body is divided into the toilet and filter chamber being distributed up and down by the card, Cage bone is installed on the card, is cased with filter bag on the cage bone；The side wall of the toilet be equipped with net gas outlet and nitrogen into Mouthful, the bottom of the tank body offers fuel gas and dust import, and the filter chamber is communicated with the fuel gas and dust import；Wherein, institute Stating filter further includes pulse of nitrogen blowing device, and the pulse control instrument of the control pulse of nitrogen blowing device, described Pulse of nitrogen blowing device includes nitrogen inlet, solenoid valve, multiple injection tubes and nozzle；The pulse of nitrogen blowing device installation There are multiple solenoid valves, each solenoid valve is used to control the opening and closing of nitrogen in an injection tube, and the injection tube passes through described The cylinder of solenoid valve is connected to the nitrogen inlet, and the injection tube is equipped with multiple nozzles, and the mouthpiece of the nozzle is located at institute The surface of filter pocket openings is stated, the solenoid valve is electrically connected with the pulse control instrument.

9. the silicon tetrachloride slag slurry processing method in a kind of cold hydrogenation process characterized by comprising

(1) silicon tetrachloride slag slurry for generating cold hydrogenation process imports dry blender as claimed in any one of claims 1 to 6 In, the silicon tetrachloride slag slurry is heated in the dry blender, is stirred, chlorosilane gas is isolated and slurry is solid Body object；

(2) chlorosilane gas enters in the filter of the dry whip topping, and the filter is to the chlorosilane Gas is filtered, and the dust that the chlorosilane gas is taken out of is attracted on the filter bag of the filter, and it is clean to obtain chlorosilane Net gas, under the blowing of the filter, the dust being adsorbed on filter bag is fallen into the dry blender；

(3) the chlorosilane clean gas enters the chlorosilane recycling being connected with the filter, and is condensed into chlorine silicon Alkane liquid, the chlorosilane liquid produced are recycled for being delivered in cold hydrogenation process；

(4) the slurry solids is expelled in washing packet with the dust for falling into dry blender, is wrapped in the washing In, neutralization reaction is hydrolyzed in the slurry solids and the dust and lye, and the solid-liquid after the neutralization reaction is mixed Object discharge.