CN106927470A - The recovery method of chlorosilane waste liquid - Google Patents
The recovery method of chlorosilane waste liquid Download PDFInfo
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- CN106927470A CN106927470A CN201710237329.3A CN201710237329A CN106927470A CN 106927470 A CN106927470 A CN 106927470A CN 201710237329 A CN201710237329 A CN 201710237329A CN 106927470 A CN106927470 A CN 106927470A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10778—Purification
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Abstract
The invention provides a kind of recovery method of chlorosilane waste liquid.The recovery method includes：Chlorosilane waste liquid is spray-dried, gas-solid mixture is obtained, chlorosilane waste liquid is included silicon tetrachloride liquid, silica flour, aluminium chloride, iron chloride and titanium chloride；And gas-solid mixture is carried out into gas solid separation, obtain thick chlorosilane gas and solid slag.Above-mentioned recovery method can be reclaimed to chlorosilane waste liquid at low cost, realize the clean manufacturing of polysilicon, reduce the discharge of cost of investment and chlorion, and remarkable in economical benefits is environment-friendly, thus the technique has excellent economical and environmentally friendly benefit.
Description
Technical field
The present invention relates to field of polysilicon production, in particular to a kind of recovery method of chlorosilane waste liquid.
Background technology
Silicon tetrachloride cold hydrogenation system, trichlorosilane synthesis system or rectifying and purifying system in polycrystalline silicon preparing process are led to
A certain amount of chlorosilane waste liquid can be often discharged, substantial amounts of chlorosilane is contained in raffinate, also contain trickle silica flour and metal chlorination
Thing.Because containing silica flour and metal chloride, chlorosilane waste liquid is easy to occluding device and pipeline.If chlorosilane given up simultaneously
Liquid directly outer row's treatment, not only results in the loss of chlorosilane, and acid mist is easily formed after chlorosilane can also contacted with air or water
Pollution environment.So that being reclaimed to chlorosilane in the chlorosilane waste liquid of generation in polysilicon production process.
Mainly there are Hydrolyze method, filtration method, burning method and evaporation for the recovery method of chlorosilane waste liquid both at home and abroad.
Hydrolyze method is the method that domestic polysilicon enterprise generally uses, and concrete technology is that chlorosilane gives up in hydrolysis device
Liquid is passed through in water the reaction that is hydrolyzed, and obtains the waste water and silica solid slag of hydrogen chloride gas and acidity, then hydrogen chloride gas
Body is reclaimed after tail gas drip washing and condensation process, and silica solid slag is directly filled or utilized after simple neutralisation treatment.Due to
Raffinate amount is larger, and the method generates substantial amounts of acid waste water and hydrolysis residue, thus its three-protection design load is larger, environmental pollution
Also it is very serious.
Filtration method is the impurity such as solid dust and metal chloride in filtering raffinate by filter by raffinate, is obtained
The filtrate arrived recycles.The method has reclaimed chlorosilane to a certain extent, but trickle dust and metal chloride pole
Easily block pipeline and equipment, it is difficult to realize continuous production, maintenance difficulty is big.
Burning method is that chlorosilane waste liquid is carried out burning conversion under the high temperature conditions for silica.The method is in certain journey
The process problem of raffinate is solved on degree, but the quality of silica is not high, while producing substantial amounts of chlorination in burning process
Hydrogen, and the once investment of burning facility is higher.
Evaporation is that chlorosilane waste liquid is passed through in evaporating kettle, chlorosilane is evaporated under external heat, after condensation
Reclaimed.The method has reclaimed part chlorosilane to a certain extent, but has the disadvantage the disposal ability very little of evaporating kettle, blocks
Seriously, and heat transfer effect is not good, energy consumption is higher.
The content of the invention
It is a primary object of the present invention to provide a kind of recovery method of chlorosilane waste liquid, given up with solving existing chlorosilane
The problem of the recovery method feature of environmental protection difference of liquid.
To achieve these goals, one aspect of the invention provides a kind of recovery method of chlorosilane waste liquid, recovery side
Method includes：Chlorosilane waste liquid is spray-dried, gas-solid mixture is obtained, chlorosilane waste liquid is included silicon tetrachloride liquid, silicon
Powder, aluminium chloride, iron chloride and titanium chloride；And gas-solid mixture is carried out into gas solid separation, obtain thick chlorosilane gas and solid slag.
Further, recovery method also includes：Before the process being spray-dried, first chlorosilane waste liquid is steamed
Hair, obtains chlorosilane gas and steams extraction raffinate；And spray-drying process is carried out by extraction raffinate is steamed, obtain gas-solid mixture.
Further, the temperature of evaporation process is 55~100 DEG C, and evaporation gauge pressure is 0~0.3Mpa (g).
Further, recovery method also includes：Before process is evaporated, by chlorosilane waste liquid and complexing agent sodium chloride
After mixing, filtrate and filter residue are filtrated to get；And filtrate is evaporated process, obtain chlorosilane gas and steam extraction raffinate.
Further, spray-drying process also includes：Carrier gas is carried out to be heated to 150~250 DEG C, obtains heating carrier gas；
And spray-drying process is carried out in the presence of carrier gas is heated, obtain gas-solid mixture.
Further, carrier gas is selected from nitrogen.
Further, thick chlorosilane gas and chlorosilane gas are condensed, is obtained chlorosilane liquid produced.
Further, when spray-drying process is carried out in the presence of heating carrier gas, the product of condensation process is also included not
Solidifying gas, recycles fixed gas as carrier gas.
Further, the method for gas solid separation is to be constituted using rotoclone collector, filtering type dust-precipitator and cottrell
Carry out gas solid separation one or more in group.
Apply the technical scheme of the present invention, chlorosilane waste liquid can be reclaimed at low cost, realize polysilicon
Clean manufacturing, reduce the discharge of cost of investment and chlorion, remarkable in economical benefits is environment-friendly, thus the technique has excellent
Different economical and environmentally friendly benefit.
Brief description of the drawings
The Figure of description for constituting the part of the application is used for providing a further understanding of the present invention, of the invention to show
Meaning property and its illustrates, for explaining the present invention, not constitute inappropriate limitation of the present invention embodiment.In the accompanying drawings：
Fig. 1 shows a kind of knot of preferred embodiment middle chlorosilane Mead-Bauer recovery system for using of the invention
Structure schematic diagram.
Wherein, above-mentioned accompanying drawing is marked including the following drawings：
10th, feed unit；11st, chlorosilane waste liquid feeding mechanism；111st, waste liquid outlet；12nd, vaporising device；121st, waste liquid enters
Mouthful；122nd, extraction raffinate outlet is steamed；123rd, chlorosilane gas outlet；13rd, the first filter；131st, liquid-phase outlet；14th, complexing agent is thrown
Material device；141st, dog-house；15th, extraction raffinate storage tank is steamed；
20th, carrier gas heating unit；21st, carrier gas feeding mechanism；22nd, heater；
30th, spray-drying installation；31st, charging aperture；32nd, carrier gas inlet；33rd, gas-solid mixture outlet；
40th, gas solid separation unit；41st, cyclone separator；411st, gas-solid mixture entrance；412nd, rotation point gas vent；
42nd, the second filter；421st, rotation point gas access；422nd, thick chlorosilane gas outlet；
50th, condensing unit；51st, condensing unit；511st, thick chlorosilane gas entrance；512nd, chlorosilane liquid produced outlet；513、
Fixed gas is exported；52nd, chlorosilane liquid produced storage tank；521st, chlorosilane liquid produced entrance；53rd, tail gas condensation device；54th, dedusting dress
Put；541st, dust outlet.
Specific embodiment
It should be noted that in the case where not conflicting, the feature in embodiment and embodiment in the application can phase
Mutually combination.Describe the present invention in detail below with reference to the accompanying drawings and in conjunction with the embodiments.
As described by background technology, the existing recovery method to chlorosilane waste liquid has that the feature of environmental protection is poor to ask
Topic.In order to solve the above-mentioned technical problem, the invention provides a kind of recovery method of chlorosilane waste liquid, it includes：By chlorosilane
Waste liquid is spray-dried, and obtains gas-solid mixture, and chlorosilane waste liquid includes silicon tetrachloride liquid, silica flour, aluminium chloride, iron chloride
And titanium chloride；And gas-solid mixture is carried out into gas solid separation, obtain thick chlorosilane gas and solid slag.
Because chlorosilane waste liquid is a kind of mixture, and the boiling point difference of each component causes the volatility of each component with one
Fixed otherness.Chlorosilane waste liquid is spray-dried, chlorosilane liquid produced is rapidly evaporated to gaseous chlorosilane, so as to obtain
Chlorosilane gas-solid mixture.Then above-mentioned gas-solid mixture is carried out into gas solid separation process so as to obtain thick chlorosilane gas and sink
The solid slag (metal chloride and silicon powder particle) for lowering.
The chlorosilane method for recovering waste liquid that the application is provided, it is adaptable to separation of solid and liquid, realizes the pollution-free treatment of waste residue；
And the condition such as pressure, the temperature in above-mentioned technical process is more gentle, it is easy to safety in production, stable operation；Equipment and materials is selected
The convenient, design of equipment and processing and manufacturing are simple, disposably put into small；The low advantage of high degree of automation, maintenance cost.Using
Above-mentioned recovery method treatment chlorosilane waste liquid can at low cost realize the recovery of chlorosilane waste liquid, realize polysilicon cleaning
Production, reduces the discharge of cost of investment and chlorion, and remarkable in economical benefits is environment-friendly, thus the technique has excellent warp
Ji and environmental benefit.
The chlorosilane recovery method provided using the application carries out treatment to chlorosilane waste liquid has low cost, environment-friendly
With the advantage of high financial profit.In one kind preferred embodiment, recovery method also includes：The process being spray-dried it
Before, first chlorosilane waste liquid is evaporated, obtain chlorosilane gas and steam extraction raffinate；And spray-drying process is carried out by extraction raffinate is steamed,
Obtain gas-solid mixture.
Before being spray-dried, first chlorosilane waste liquid is evaporated and tentatively can reclaim one from chlorosilane waste liquid
Part chlorosilane gas, so as to be conducive to improving the rate of recovery of chlorosilane gas.It is preferred that constantly being stirred in above-mentioned evaporation process
Mix.The disengagement area for being conducive to improving chlorosilane waste liquid is constantly stirred in evaporation process, so as to be conducive to further raising
The rate of recovery of evaporation effect and chlorosilane gas.
In above-mentioned recovery method, the temperature and time of evaporation process can select the temperature that chlorosilane can arbitrarily evaporated
Degree and time.Preferred embodiment the temperature of evaporation process is 55~100 DEG C a kind of, in evaporator gauge pressure control 0~
0.3Mpa(g).The temperature and time of evaporation process is limited and is conducive to further improving chlorine in evaporation process within the above range
The evaporation efficiency of silane.
In one kind preferred embodiment, above-mentioned recovery method also includes：Before being evaporated, by chlorosilane waste liquid with
After the mixing of complexing agent sodium chloride, filtrate and filter residue are filtrated to get；And be evaporated above-mentioned filtrate, obtain chlorosilane gas and steaming
Extraction raffinate.
As it was noted above, containing a certain amount of metal chloride in chlorosilane waste liquid, concrete composition see the table below 1.
Table 1
Larger mainly aluminium chloride is wherein influenceed, if not removing it easy occluding device and pipeline.In order to solve
Above mentioned problem, the chlorosilane method for recovering waste liquid that the application is provided is by complexing agent is put into chlorosilane waste liquid, making above-mentioned gold
Category chloride occur complex reaction after from chlorosilane waste liquid separate out, then again through filter process by above-mentioned complex compound from waste liquid
Removing.This greatly reduces AlCl3The partial pressure of gas phase in filter so that AlCl3In resting on the slag phase of filter,
So as to advantageously reduce AlCl3Subsequent evaporation condensation deposition reduces the frequency of parking maintenance to equipment, the risk of the blocking of pipeline
Rate, also helps the range of choice of carrier gas temperature in subsequent cell.Simultaneously because through filter process, it is impossible to by the solid in waste liquid
Impurity is removed completely, thus above-mentioned filtrate obtains still also having a small amount of solid slag in steaming extraction raffinate after pervaporation.Above-mentioned complexing agent with
Metal chloride in chlorosilane waste liquid has more excellent complex performance, thus favourable as complexing agent from above-claimed cpd
The removal efficiency of metal chloride in chlorosilane waste liquid is improved.
In above-mentioned recovery method, the heating-up temperature of carrier gas can any chlorosilane can be made to convert gaseous temperature by liquid
Degree.In one kind preferred embodiment, spray-drying process also includes：Carrier gas is carried out to be heated to 150~250 DEG C, is added
Hot carrier gas；And spray-drying process is carried out in the presence of carrier gas is heated, obtain gas-solid mixture.The temperature of carrier gas is heated to
Said temperature scope is conducive to improving the efficiency of spray-drying process, while accessory substance is less.It is preferred that carrier gas is included but is not limited to
Nitrogen and/or inert gas.
Preferred embodiment thick chlorosilane gas and chlorosilane gas are condensed a kind of, obtained chlorosilane liquid
Body.Thick chlorosilane gas cool down and is conducive to separating more pure chlorosilane gas, while by chlorosilane gas
Body is conducive to it to transport and store after being cooled to liquid.
In one kind preferred embodiment, the product of above-mentioned condensation process also includes carrier gas, in the presence of carrier gas is heated
When carrying out spray-drying process, the product of condensation process also includes fixed gas, and profit is circulated using above-mentioned fixed gas as the carrier gas
With.It is carrier gas by above-mentioned fixed gas, is circulated utilization, advantageously reduces process costs.
In one kind preferred embodiment, the chlorosilane gas obtained through evaporation process carry out gas and remove before being condensed
Dirt process, this is conducive to improving the purity of the chlorosilane liquid produced being recovered to；To more preferably be collected in above-mentioned gas dust removal process
To dust deliver to follow-up gas solid separation process and focused on, this advantageously reduces the working strength of operating personnel.
In above-mentioned recovery method, the method for gas solid separation can select the conventional gas-solid separating method in this area.In one kind
Preferred embodiment, the method for gas solid separation includes but is not limited to be gathered dust using rotoclone collector, filtering type dust-precipitator and electricity
Carry out above-mentioned gas solid separation process one or more in the group of device composition.It is preferred that gas solid separation process is first to mix above-mentioned gas-solid
Compound carries out cyclonic separation, and pocket filtering is then carried out again.The method being superimposed using above two separate mode carries out above-mentioned gas
Solid separation process is conducive to further improving the separative efficiency of gas solid separation process, and then is conducive to improving the purity of chlorosilane.
In order to be better understood from above-mentioned recovery method, this application provides the device that a kind of preferred chlorosilane is reclaimed, such as
Shown in Fig. 1, specific removal process is as follows：
The device that chlorosilane is reclaimed mainly includes feed unit 10, carrier gas heating unit 20, spray-drying installation 30, gas-solid
Separative element and cooling unit.Chlorosilane raffinate is by the waste liquid outlet 111 of chlorosilane waste liquid feeding mechanism 11 through chlorosilane waste liquid
Transfer pipeline is delivered to the first filter 13, and complexing agent was first passed through before above-mentioned first filter 13 is entered feeds intake dress
14 are put to consolidate to complexing agent sodium chloride nacl is put into the chlorosilane waste liquid in above-mentioned chlorosilane waste liquid transfer pipeline through dog-house 141
Body, solid slag such as silica flour, metal chloride, mainly AlCl are obtained after being filtered through the first filter 133Enter into slag phase and filter
Liquid.
Above-mentioned filtrate is delivered into waste liquid entrance 121 through liquid-phase outlet 131 to be evaporated into vaporising device 12, is steamed
Extraction raffinate and chlorosilane gas.Then above-mentioned steaming extraction raffinate is delivered to charging aperture 31 into spray drying dress through steaming extraction raffinate outlet 122
Put 30 to be spray-dried, obtain gas-solid mixture.Then above-mentioned gas-solid mixture is delivered to through gas-solid mixture outlet 33
Gas-solid mixture entrance 411 enters the cyclone separator 41 (rotoclone collector) of gas solid separation unit 40, obtains rotation point gas.
Rotation point gas is delivered to rotation point gas access 421 and enters (the filtering type dust-precipitator of the second filter 42 through rotation point gas vent 412
Or cottrell) gas solid separation is carried out, obtain thick silane gas and solid slag.It is preferred that being filled in above-mentioned gas solid separation unit 40 and evaporation
Set between putting 12 and steam extraction raffinate storage tank 15.It is preferred that carrier gas heating unit 20 includes carrier gas feeding mechanism 21 and heater 22, warp
Carrier gas after heating enters in spray-drying installation 30 through carrier gas inlet 32, for providing thermal source for spray-drying installation 30.
Above-mentioned thick silane gas are delivered to thick chlorosilane gas entrance 511 and enter condensation through thick chlorosilane gas outlet 422
Condensed in the condensing unit 51 of unit 50, obtained chlorosilane liquid produced and fixed gas.By above-mentioned chlorosilane liquid produced through chlorosilane
Liquid inlet 521 is stored in chlorosilane liquid produced storage tank 52.It is preferred that above-mentioned fixed gas is returned into carrier gas through fixed gas outlet 513 adding
Hot cell 20 is circulated utilization as carrier gas.Above-mentioned vaporising device 12 is obtained chlorosilane gas simultaneously are by chlorosilane gas
Body outlet 123 exports 512 through chlorine silicon after being delivered to gas dust-removing device 54 and tail gas condensation device 53 successively by chlorosilane liquid produced
Alkane liquid inlet 521 is delivered in chlorosilane liquid produced storage tank 52, and the dust in gas dust-removing device 54 is conveyed through dust outlet 541
To vaporising device 12.
The application is described further with reference to embodiment.
Chlorosilane raffinate of the chlorosilane waste liquid from the cold hydrogenation chilling tower bottoms of fluid bed in embodiment 1 to 8, wherein
SiCl4Account for 70% (wt), high-boiling components and be mainly Si2Cl6Account for 20% (wt), metal chloride and silica flour and account for 10% (wt), gross mass
Flow is 3000kg/h, and feeding temperature is 40 DEG C, and feed pressure is 0.1MPa (g).
Embodiment 1
Above-mentioned chlorosilane waste liquid is evaporated, obtains steaming extraction raffinate and chlorosilane gas, evaporation process temperature is 70 DEG C, is steamed
Pressure is delivered for 0.1MPa (g).
After above-mentioned chlorosilane waste liquid is spray-dried (carrier gas is nitrogen), gas-solid mixture is obtained, spray drying
Temperature is 220 DEG C.
Then above-mentioned gas-solid mixture is carried out into gas solid separation and obtains thick silane gas and solid slag, the rate of recovery of thick silane is
SiCl4And Si2Cl6The rate of recovery >=88%, slag phase water capacity≤4% (wt) after drying.
Embodiment 2
Above-mentioned chlorosilane waste liquid is evaporated, obtains steaming extraction raffinate and chlorosilane gas, evaporation process temperature is 100 DEG C,
Evaporation gauge pressure is 0.1MPa (g).
After above-mentioned steaming extraction raffinate is spray-dried (carrier gas is nitrogen), gas-solid mixture, the temperature of spray drying are obtained
It is 220 DEG C.
Then above-mentioned gas-solid mixture is carried out into gas solid separation and obtains thick silane gas and solid slag, the rate of recovery of thick silane is
SiCl4And Si2Cl6The rate of recovery >=90%, slag phase water capacity≤4% (wt) after drying.
Embodiment 3
Above-mentioned chlorosilane waste liquid is evaporated, obtains steaming extraction raffinate and chlorosilane gas, evaporation process temperature is 100 DEG C,
Evaporation gauge pressure is 0.2MPa (g).
After above-mentioned steaming extraction raffinate is spray-dried (carrier gas is nitrogen), gas-solid mixture, the temperature of spray drying are obtained
It is 220 DEG C.
Then above-mentioned gas-solid mixture is carried out into gas solid separation and obtains thick silane gas and solid slag, the rate of recovery of thick silane is
SiCl4And Si2Cl6The rate of recovery >=92%, slag phase water capacity≤4% (wt) after drying.
Embodiment 4
Above-mentioned chlorosilane waste liquid is evaporated, obtains steaming extraction raffinate and chlorosilane gas, evaporation process temperature is 55 DEG C, is steamed
Pressure is delivered for 0.2MPa.
After above-mentioned steaming extraction raffinate is spray-dried (carrier gas is nitrogen), gas-solid mixture, the temperature of spray drying are obtained
It is 220 DEG C.
Then above-mentioned gas-solid mixture is carried out into gas solid separation and obtains thick silane gas and solid slag, the rate of recovery of thick silane is
SiCl4And Si2Cl6The rate of recovery >=87%, slag phase water capacity≤4% (wt) after drying.
Embodiment 5
To complexing agent sodium chloride is added in above-mentioned chlorosilane waste liquid, filtrate and solid slag are filtrated to get, its complexing agent chlorination
Sodium is more than 1 with the weight ratio of chlorosilane waste liquid.
(carrier gas is nitrogen) is evaporated with by above-mentioned chlorosilane waste liquid, obtains steaming extraction raffinate and chlorosilane gas, evaporated
Cheng Wendu is 100 DEG C, and evaporation gauge pressure is 0.2MPa.
After above-mentioned steaming extraction raffinate is spray-dried, gas-solid mixture is obtained, the temperature of spray drying is 220 DEG C.
Then above-mentioned gas-solid mixture is carried out into gas solid separation and obtains thick silane gas and solid slag, the rate of recovery of thick silane is
SiCl4And Si2Cl6The rate of recovery >=94%, slag phase water capacity≤4% (wt) after drying.
Embodiment 6
Above-mentioned chlorosilane waste liquid is evaporated, obtains steaming extraction raffinate and chlorosilane gas, evaporation process temperature is 100 DEG C,
Evaporation gauge pressure is 0.2MPa.
After above-mentioned steaming extraction raffinate is spray-dried (carrier gas is nitrogen), gas-solid mixture, the temperature of spray drying are obtained
It is 150 DEG C.
Then above-mentioned gas-solid mixture is carried out into gas solid separation and obtains thick silane gas and solid slag, the rate of recovery of thick silane is
SiCl4And Si2Cl6The rate of recovery >=89%, slag phase water capacity≤6% (wt) after drying
Embodiment 7
Above-mentioned chlorosilane waste liquid is evaporated, obtains steaming extraction raffinate and chlorosilane gas, evaporation process temperature is 100 DEG C,
Evaporation gauge pressure is 0.2MPa.
After above-mentioned steaming extraction raffinate is spray-dried (carrier gas is nitrogen), gas-solid mixture, the temperature of spray drying are obtained
It is 250 DEG C.
Then above-mentioned gas-solid mixture is carried out into gas solid separation and obtains thick silane gas and solid slag, the rate of recovery of thick silane is
SiCl4And Si2Cl6The rate of recovery >=96%, slag phase water capacity≤3% (wt) after drying.
Embodiment 8
Above-mentioned chlorosilane waste liquid is evaporated, obtains steaming extraction raffinate and chlorosilane gas, evaporation process temperature is 100 DEG C,
Evaporation gauge pressure is 0.2MPa.
After above-mentioned steaming extraction raffinate is spray-dried (carrier gas is nitrogen), gas-solid mixture, the temperature of spray drying are obtained
It is 130 DEG C.
Then above-mentioned gas-solid mixture is carried out into gas solid separation and obtains thick silane gas and solid slag, the rate of recovery of thick silane is
SiCl4And Si2Cl6The rate of recovery >=70%, slag phase water capacity≤13% (wt) after drying.
Seen from the above description, the application realizes following technique effect：Chlorosilane waste liquid can be entered at low cost
Row is reclaimed, and realizes the clean manufacturing of polysilicon, reduces the discharge of cost of investment and chlorion, remarkable in economical benefits.Simultaneously
Above-mentioned whole technological process is carried out including material filtering, evaporation process etc. in closed environment, so as to effectively prevent
The leakage of material, whole flow process realizes continuous prodution.
The preferred embodiments of the present invention are the foregoing is only, is not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.It is all within the spirit and principles in the present invention, made any repair
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (9)
1. a kind of recovery method of chlorosilane waste liquid, it is characterised in that the recovery method includes：
The chlorosilane waste liquid is spray-dried, gas-solid mixture is obtained, the chlorosilane waste liquid is included silicon tetrachloride liquid
Body, silica flour, aluminium chloride, iron chloride and titanium chloride；And
The gas-solid mixture is carried out into gas solid separation, thick chlorosilane gas and solid slag is obtained.
2. recovery method according to claim 1, it is characterised in that the recovery method also includes：
Before the process of the spray drying is carried out, first the chlorosilane waste liquid is evaporated, obtain chlorosilane gas and
Steam extraction raffinate；And
The steaming extraction raffinate is carried out into the spray-drying process, the gas-solid mixture is obtained.
3. recovery method according to claim 2, it is characterised in that the temperature of the evaporation process is 55~100 DEG C, is steamed
Pressure is delivered for 0~0.3MPa.
4. recovery method according to claim 2, it is characterised in that the recovery method also includes：
Before the evaporation process is carried out, after the chlorosilane waste liquid is mixed with complexing agent sodium chloride, filtrate is filtrated to get
And filter residue；And
The filtrate is carried out into the evaporation process, the chlorosilane gas and the steaming extraction raffinate is obtained.
5. recovery method according to any one of claim 1 to 4, it is characterised in that the spray-drying process is also wrapped
Include：
Carrier gas is heated to 150~250 DEG C, obtains heating carrier gas；And
The spray-drying process is carried out in the presence of the heating carrier gas, the gas-solid mixture is obtained.
6. recovery method according to claim 5, it is characterised in that the carrier gas is selected from nitrogen.
7. recovery method according to claim 5, it is characterised in that by the thick chlorosilane gas and the chlorosilane gas
Body is condensed, and obtains chlorosilane liquid produced.
8. recovery method according to claim 7, it is characterised in that carry out the spray in the presence of the heating carrier gas
During mist drying process, the product of the condensation process also includes fixed gas, is recycled the fixed gas as the carrier gas.
9. recovery method according to claim 1, it is characterised in that the method for the gas solid separation is to use cyclone dust collection
Carry out the gas solid separation one or more in the group of device, filtering type dust-precipitator and cottrell composition.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109077063A (en) * | 2018-08-16 | 2018-12-25 | 乐山师范学院 | A kind of titania-silica micro mist and its preparation method and application |
| WO2020215706A1 (en) * | 2019-04-26 | 2020-10-29 | 天津科技大学 | Chlorosilane high-boiling residue recovery process combining slurry treatment and cracking reaction |
| CN112408396A (en) * | 2020-11-30 | 2021-02-26 | 天津大学 | Process and equipment for removing aluminum by chlorosilane complexation |
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| US6090360A (en) * | 1995-02-15 | 2000-07-18 | Dow Corning Corporation | Method for recovering particulate silicon from a by-product stream |
| CN102372271A (en) * | 2011-08-17 | 2012-03-14 | 乐山乐电天威硅业科技有限责任公司 | Recovery method of waste chlorsilane in polysilicon produced through modified Simens Method |
| CN102602936A (en) * | 2012-03-14 | 2012-07-25 | 天津大学 | Method and device for treating residual silicon tetrachloride liquor |
| CN102942183A (en) * | 2012-12-11 | 2013-02-27 | 成都蜀菱科技发展有限公司 | Chlorosilane raffinate treating technology |
| CN105480980A (en) * | 2014-09-17 | 2016-04-13 | 新特能源股份有限公司 | Method and device for treating residue slurry resulting from trichlorosilane production |
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| CN109077063A (en) * | 2018-08-16 | 2018-12-25 | 乐山师范学院 | A kind of titania-silica micro mist and its preparation method and application |
| CN109077063B (en) * | 2018-08-16 | 2021-02-12 | 乐山师范学院 | Titanium dioxide-silicon dioxide micro powder and preparation method and application thereof |
| WO2020215706A1 (en) * | 2019-04-26 | 2020-10-29 | 天津科技大学 | Chlorosilane high-boiling residue recovery process combining slurry treatment and cracking reaction |
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