CN109292781A - A kind of method and device using organosilicon silicon slag production chlorosilane - Google Patents
A kind of method and device using organosilicon silicon slag production chlorosilane Download PDFInfo
- Publication number
- CN109292781A CN109292781A CN201811333009.9A CN201811333009A CN109292781A CN 109292781 A CN109292781 A CN 109292781A CN 201811333009 A CN201811333009 A CN 201811333009A CN 109292781 A CN109292781 A CN 109292781A
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- China
- Prior art keywords
- gas
- cooling
- silicon slag
- chlorosilane
- reaction gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002893 slag Substances 0.000 title claims abstract description 125
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 239000010703 silicon Substances 0.000 title claims abstract description 107
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 107
- 239000005046 Chlorosilane Substances 0.000 title claims abstract description 70
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 54
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 43
- 238000001816 cooling Methods 0.000 claims abstract description 131
- 238000002156 mixing Methods 0.000 claims abstract description 95
- 239000012495 reaction gas Substances 0.000 claims abstract description 74
- 239000007789 gas Substances 0.000 claims abstract description 61
- 239000011261 inert gas Substances 0.000 claims abstract description 32
- 239000007787 solid Substances 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000460 chlorine Substances 0.000 claims abstract description 11
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 11
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 11
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002347 injection Methods 0.000 claims description 38
- 239000007924 injection Substances 0.000 claims description 38
- 239000000047 product Substances 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 15
- 229910001510 metal chloride Inorganic materials 0.000 claims description 14
- 239000011343 solid material Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000004891 communication Methods 0.000 claims description 5
- SBEQWOXEGHQIMW-UHFFFAOYSA-N silicon Chemical compound [Si].[Si] SBEQWOXEGHQIMW-UHFFFAOYSA-N 0.000 claims description 4
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims description 4
- 239000005052 trichlorosilane Substances 0.000 claims description 4
- 230000004044 response Effects 0.000 claims description 3
- 239000012263 liquid product Substances 0.000 claims description 2
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 125000001309 chloro group Chemical group Cl* 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 16
- 239000002826 coolant Substances 0.000 description 21
- 230000007717 exclusion Effects 0.000 description 14
- 230000008676 import Effects 0.000 description 9
- 230000007246 mechanism Effects 0.000 description 8
- 239000002699 waste material Substances 0.000 description 7
- 238000010586 diagram Methods 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 5
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000498 cooling water Substances 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000005049 silicon tetrachloride Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 210000000481 breast Anatomy 0.000 description 3
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 3
- 239000000112 cooling gas Substances 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- POFAUXBEMGMSAV-UHFFFAOYSA-N [Si].[Cl] Chemical compound [Si].[Cl] POFAUXBEMGMSAV-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003818 cinder Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- -1 alchlor Chemical compound 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003434 inspiratory effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- 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
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
- C01B33/10715—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by reacting chlorine with silicon or a silicon-containing material
- C01B33/10721—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by reacting chlorine with silicon or a silicon-containing material with the preferential formation of tetrachloride
- C01B33/10726—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by reacting chlorine with silicon or a silicon-containing material with the preferential formation of tetrachloride from silicon
-
- 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
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
- C01B33/10715—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by reacting chlorine with silicon or a silicon-containing material
- C01B33/10731—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by reacting chlorine with silicon or a silicon-containing material with the preferential formation of trichlorosilane
- C01B33/10736—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by reacting chlorine with silicon or a silicon-containing material with the preferential formation of trichlorosilane from silicon
-
- 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
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
- C01B33/10742—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material
- C01B33/10747—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of tetrachloride
- C01B33/10752—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of tetrachloride from silicon
-
- 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
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
- C01B33/10742—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material
- C01B33/10757—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane
- C01B33/10763—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane from silicon
Abstract
The invention discloses a kind of method and devices using organosilicon silicon slag production chlorosilane, are related to organic silicon technology field.This includes: to pass through that silicon slag feed inlet and reaction gas feed inlet is made to generate negative pressure in mixing arrangement high speed using inert gas using the method that organosilicon silicon slag produces chlorosilane, and then it is uniformly mixed silicon slag and reaction gas in mixing arrangement, wherein, the flow velocity of inert gas is 100-300m/s, and reaction gas is hydrogen chloride or chlorine；Mixed gas is reacted under the conditions of 240-350 DEG C of temperature, tentatively cooling under the conditions of 130-160 DEG C of temperature, then secondary cooling obtains chlorosilane gas under the conditions of 70-130 DEG C of temperature.It is device for implementing the above method that this, which utilizes the device of organosilicon silicon slag production chlorosilane, realizes being sufficiently mixed for silicon slag and reaction gas by improving gas-solid mixing device, and then by obtaining chlorosilane product after reaction and removal of impurities.
Description
Technical field
The present invention relates to organosilicon technical fields, and in particular to a kind of method using organosilicon silicon slag production chlorosilane
And device.
Background technique
In recent years, with the continuous development of domestic economy, silicone industry is rapidly developed.With organic silicon monomer first
The raising at full speed of base chlorosilane production capacity, the quantity of by-product are also increasing；If dealt with improperly, environment is not only endangered, also will
Seriously affect the sound development of silicone industry.It is reported that the waste that now external every production 100kg methylchlorosilane generates is
It is down to 3.5kg via the 28kg of nineteen sixty, waste has obtained good improvement；And the waste that methylchlorosilane production in China's generates
10-11kg is then reached, appropriate processing is not yet received in waste.
Silicon slag is the discarded object of power boiler discharge of direct synthesis methylchlorosilane technique, main component be silicon, copper, carbon,
Zinc etc..Silicon slag is not easy to store, and meets air and oxidation reaction occurs, make organic substance therein and carbon burning and the white of extremely difficult news of emerging
Cigarette, environmental pollution is serious, while also bringing production safety hidden danger.Domestic each scientific research institution recycles also not silicon slag processing at present
There is the research of more environmental protection and economy to report.With the production-scale continuous expansion of organosilicon, silicon slag amount can be continuously increased, how right
Silicon slag is rationally utilized, and is always the big bottleneck problem for restricting China's Silicone Industry.Utilizing for silicon slag exists very
More problems, Major Difficulties are the granularity of silicon slag minimum (400-800 mesh), impurity content is more, reaction is uncontrollable etc..
Summary of the invention
The purpose of the present invention is to provide a kind of methods using organosilicon silicon slag production chlorosilane, it is intended to raw using silicon slag
Chlorosilane is produced, realization is turned waste into wealth.
Another object of the present invention is to provide a kind of devices using organosilicon silicon slag production chlorosilane, can be realized
The conveying of the minimum silicon slag of partial size, and it is uniformly mixed silicon slag and reaction gas, and then by raw with chlorine or hcl reaction
Produce chlorosilane product.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The invention proposes a kind of methods using organosilicon silicon slag production chlorosilane, include the following steps:
Being passed through using inert gas in mixing arrangement high speed makes silicon slag feed inlet and reaction gas feed inlet generate negative pressure,
And then it is uniformly mixed silicon slag and reaction gas in mixing arrangement, wherein the flow velocity of inert gas is 100-300m/s, reaction
Gas is hydrogen chloride or chlorine；
Mixed gas is reacted under the conditions of 240-350 DEG C of temperature, it is preliminary cold under the conditions of 130-160 DEG C of temperature
But, then secondary cooling obtains chlorosilane gas under the conditions of 70-130 DEG C of temperature.
The present invention also proposes a kind of device using organosilicon silicon slag production chlorosilane, utilizes organosilicon silicon slag for above-mentioned
The method for producing chlorosilane, including the raw material conveying device, gas-solid mixing device, heating response device, primary cooling set gradually
Device, secondary coolers and product purifying device；
Raw material conveying device includes inert gas delivery pipe and reaction letter shoot；
Gas-solid mixing device includes the injection pipe that mixed charge and caliber are less than mixed charge, and one end of injection pipe is located at mixed
It is external to close supervisor, and the other end of injection pipe stretches in mixed charge；
Be provided with reaction gas feed inlet and solid material feed inlet on mixed charge, the outlet of inert gas delivery pipe with
The inlet communication of injection pipe, the outlet for reacting letter shoot are connected to reaction gas feed inlet.
The beneficial effect that the embodiment of the present invention provides a kind of method using organosilicon silicon slag production chlorosilane is: it passes through
Negative pressure is generated in silicon slag feed inlet and reaction gas feed inlet in the current inert gas of height, makes silicon slag and reaction gas mixed
It attaches together in setting and is uniformly mixed；Silicon slag and reaction gas reaction production chlorosilane, regulating and controlling cooling temperature by step cooling makes metal
Chloride deposits removal in secondary cooling, obtains more pure chlorosilane gas.
A kind of device using organosilicon silicon slag production chlorosilane provided in an embodiment of the present invention, for above-mentioned using organic
The method that silicon silicon slag produces chlorosilane realizes being sufficiently mixed for silicon slag and reaction gas by improving gas-solid mixing device, into
And by obtaining chlorosilane product after reaction and removal of impurities.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the integrated artistic figure provided in an embodiment of the present invention that chlorosilane is produced using organosilicon silicon slag；
Fig. 2 is the structural schematic diagram of gas-solid mixing device provided in an embodiment of the present invention；
Fig. 3 is the location diagram in Fig. 2 between injection pipe and the first mixing section；
Fig. 4 is the structural schematic diagram for the gas-solid mixing system that embodiment of the present invention provides；
Fig. 5 is the structural schematic diagram for the cooling exclusion device that embodiment of the present invention provides；
Fig. 6 is the enlarged drawing in IIth area Tu5Zhong；
Fig. 7 is the structural schematic diagram for the cooling impurity removed system that invention embodiment provides；
Fig. 8 is the top view of cooling impurity removed system in Fig. 7.
Icon: 10- gas-solid mixing device；110- mixed charge；111- reaction gas feed inlet；The charging of 112- solid material
Mouthful；113- segmental arc；114- mixing section；The first mixing section of 115-；The second mixing section of 116-；117- third mixing section；118- is clear
Cinder notch；119- heating device；120- injection pipe；20- gas-solid mixing system；40- cools down exclusion device；101- cooling gas outlet；
102- cooling air import；Cooler at the top of 130-；131- cools down outer tube；132- gas passage；133- rotating mechanism；1331- turns
Moving axis；1332- helical structure；1333- driving motor；134- cooling collar；The outlet of 1342- cooling medium；1344- cooling medium
Import；The cold liquid channel 135-；Receive slag device in the bottom 140-；141- slag notch；142- top section；144- bottom stage；30- cooling system
System；150- primary cooler；151- cooling medium inlet；The outlet of 152- cooling medium；153- cooling air inner tube；154- is cooling to be situated between
Matter outer tube.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
The method and device provided in an embodiment of the present invention using organosilicon silicon slag production chlorosilane is carried out below specific
Explanation.
A kind of method using organosilicon silicon slag production chlorosilane provided in an embodiment of the present invention comprising following steps:
S1, gas-solid mixing
Being passed through using inert gas in mixing arrangement high speed makes silicon slag feed inlet and reaction gas feed inlet generate negative pressure,
And then it is uniformly mixed silicon slag and reaction gas in mixing arrangement, wherein the flow velocity of inert gas is 100-300m/s, reaction
Gas is hydrogen chloride or chlorine.Inventors have found that enabling silicon slag and reaction gas using above-mentioned principle by improving mixing arrangement
Enough realize is uniformly mixed, and provides precondition for silicon slag and reaction gas reaction.
It specifically, is 2-20kpa in the negative pressure that silicon slag feed inlet and reaction gas feed inlet generate, the generation of negative pressure guarantees
Charging and uniformly mixed condition, and the size of negative pressure is also the regulation to gas flow, and inventor has found negative pressure above-mentioned
It can make that silicon slag and reaction gas are uniformly mixed and the ratio of the two is more appropriate in range.
The dosage of reaction gas is also required to, when reaction gas is hydrogen chloride, silicon slag and reaction gas
Weight ratio be 28-56:110；When reaction gas is chlorine, the weight ratio of silicon slag and reaction gas is 27-55:140.It is general and
Speech, when synthesizing crude monomer, in its cyclone dust removal link, generating thinner silicon slag, (main component is metallic silicon for organosilicon factory
Si:80-93% contains aluminium Al:0.1- containing impurity iron Fe0.2-3% containing catalyst copper Cu and its compound 0.67-9%
0.8%, calcium Ca:0.12-1.2%, granularity is in -800 mesh of 400 mesh).The dosage of reaction gas will mutually be fitted with silicone content in silicon slag
It answers, the too low silicon slag of dosage cannot react sufficiently, and dosage is excessively high, cause the waste of reaction gas.
Preferably, if injection gas is inert gas, the injection flow of inert gas is 20-30m3/ h, slag charge charging
The revolving speed of the batcher connected at mouthful is 10-15r/min；If injection gas is reaction gas, the injection flow of reaction gas
For 15-25m3/ h, the revolving speed of the batcher connected at slag charge feed inlet are 8-12r/min.
S2, reaction
Mixed gas is reacted under the conditions of 240-350 DEG C of temperature, inventors have found that sufficiently mixed in the gas-solid mixing stage
Reaction temperature is advisable at 240-350 DEG C after conjunction, and the generation of the excessively high aggravation by-product of reaction temperature, reaction temperature is crossed low reaction and do not filled
Point.Furthermore, it is possible to be preheated before entering the reactor, to shorten the reaction time and reaction is promoted more fully to carry out.
S3, cooling removal of impurities
Tentatively cooling under the conditions of 130-160 DEG C of temperature, then secondary cooling obtains under the conditions of 70-130 DEG C of temperature
To chlorosilane gas.Metal chloride is still gaseous state after tentatively cooling down, and metal chloride deposits in secondary cooling process
Get off, only more pure chlorosilane gas enters subsequent handling.
Preferably, the metal chloride being deposited in cooler is collected after secondary cooling process, in secondary cooling mistake
Metal chloride constantly deposits in journey, and inventor realizes the collection of metal chloride by improving the device of secondary cooling, please join
Narration of the book about cooling exclusion device as directed.
S4, purification
This some processes can according to need progress, and the chlorosilane gas after secondary cooling needs to obtain by multistage cooling
Silicon tetrachloride or trichlorosilane liquid product, specifically, multistage cooling procedure include the temperature by chlorosilane gas at 25-35 DEG C
Under the conditions of it is cooling after, using -20~-25 DEG C of deep cooling.
Preferably, the product liquid obtained after multistage cooling is steamed into product liquid under the conditions of 100-105 DEG C of temperature,
Then it is cooled down under the conditions of 25-35 DEG C of temperature, deep cooling under the conditions of -20~-25 DEG C of temperature, eventually passes through rectifying separation.
You need to add is that realizing the purification of chlorosilane by processes such as multistage cooling, residual night recycling, this some processes can
Referring to the existing technique purified about chlorosilane.
Incorporated by reference to Fig. 1, the embodiment of the present invention provides a kind of device using organosilicon silicon slag production chlorosilane, for implementing
It is above-mentioned using organosilicon silicon slag production chlorosilane method, including set gradually raw material conveying device, gas-solid mixing device, plus
Thermal reactor, primary cooler, secondary coolers and product purifying device.Product purifying device includes multistage cooler, chlorine silicon
Residual night recyclable device of alkane etc., product purifying device, heating response device, primary cooler etc. are existing apparatus.Inventor passes through
It improves gas-solid mixing device and realizes being sufficiently mixed for silicon slag and reaction gas, pass through and improve secondary coolers (i.e. cooling removal of impurities dress
Set) realize that the collection of metal chloride removes.
Specifically, incorporated by reference to Fig. 2-Fig. 4, raw material conveying device includes inert gas delivery pipe and reacts letter shoot,
Regulating valve can be set on transfer pipeline for adjusting flow velocity, solid material can feed by loading hopper.
Specifically, gas-solid mixing device 10 includes the injection pipe 120 that mixed charge 110 and caliber are less than mixed charge 110,
One end of injection pipe 120 is located at outside mixed charge 110, and the other end of injection pipe 120 stretches in mixed charge 110；It is mixed
Close and be provided with reaction gas feed inlet 111 and solid material feed inlet 112 on supervisor 110, the outlet of inert gas delivery pipe with
The inlet communication of injection pipe 120, the outlet for reacting letter shoot are connected to reaction gas feed inlet 111.
It should be noted that gas-solid mixing device 10 provided in an embodiment of the present invention, by being inputted in injection pipe 120
Inert gas is delivered in mixed charge 110 by inert gas, makes reaction gas feed inlet using the high-speed motion of inert gas
111 and solid material feed inlet 112 generate certain negative pressure, be conducive to from two feed inlets enter solid material and gas material
It is uniformly mixed, mainly solves the problems, such as that fluidized bed is not easy to fluidize fine grained and gas.
You need to add is that the form of the casing formed using injection pipe 120 and mixed charge 110, overall operation principle
Similar to Venturi tube, higher two material inlets for enabling mixed charge 110 of gas flow rate are generated at the nozzle of injection pipe 120
Negative pressure is conducive to feed；Solid gas is mixed using the high-speed motion of inert gas after solid material and reaction gas are fed simultaneously
Uniformly.At this point, mixed charge 110 can be diversified forms, the mode being not limited in Fig. 2.
Specifically, injection pipe 120 provided in an embodiment of the present invention can adjust inspiratory capacity by control spray air flow, from
And the mixed proportion of regulating gas and solid, it is easy to operate, controllable.The inert gas that injection pipe 120 conveys can be nitrogen, helium
Gas, argon gas etc., the reaction gas that reaction gas feed inlet 111 inputs are chlorine or hydrogen chloride.
In order to reach better compounding effect, mixed charge 110 includes segmental arc 113 and mixing section 114, reaction gas into
Material mouth 111 is located at the top of segmental arc 113, and the bottom of segmental arc 113 is connected with one end of mixing section 114；Injection pipe 120 1
End is located at the outside of segmental arc 113, and the other end protrudes into mixed charge 110 from segmental arc 113 and extends to mixing section 114.
Specifically, mixing section 114 includes the first mixing section 115 and the second mixing section 116, the bottom of segmental arc 113 and the
One end of one mixing section 115 is connected, the inlet communication of the other end of the first mixing section 115 and the second mixing section 116.Second is mixed
Caliber of the caliber less than the first mixing section 115 of section 116 is closed, and the caliber of the second mixing section 116 is greater than the pipe of injection pipe 120
Diameter, solid material and gas material are mainly uniformly mixed in the second mixing section 116.
Preferably, injection pipe 120 and the first mixing section 115 are coaxial, coaxially refer to that the center line of two pipelines is overlapped.Invention
People's discovery, coaxial setting have a significant impact for the uniformity for improving material mixing.
Incorporated by reference to Fig. 2 and Fig. 3, injection pipe 120, which extends from segmental arc 113, extends to the first mixing section 115 far from segmental arc
113 one end.The outer wall of injection pipe 120 and the inner wall of the first mixing section 115 are fixed, and the stability of whole equipment is preferable.
Further, solid material feed inlet 112 is located at the top of the first mixing section 115, the bottom of the first mixing section 115
It is provided with breast hole 118.It will appear not mixed bulky grain solid in mixed process, breast hole 118 can be passed through at this time
It is collected, and gas-solid mixing device 10 is periodically discharged.
Specifically, breast hole 118 can be the pipeline extended downwardly, and seal bottom conduit, when needing that slag charge is discharged
It opens sealing and carries out deslagging.
Further, mixing section 114 further includes third mixing section 117, the import of third mixing section 117 and the second mixing section
116 outlet is connected, and the caliber of third mixing section 117 is greater than the caliber of the second mixing section 116.Third mixing section 117 is mixed
The outlet section of section 114 is closed, solid material and gas material pass through the second mixing section 116 after mixing, by third mixing section
Enter subsequent reactions section after 117 slow-downs.
Preferably, the caliber of third mixing section 117 is in the trend being gradually increased, and third mixing section 117 is close to the second mixing
The caliber of 116 one end of section is less than the caliber of the other end.Caliber by slowly increasing third mixing section 117 keeps material flow slow
It is lowered into subsequent reactions section.
Further, heating device 119 is provided on the tube wall of third mixing section 117.Heating device 119 can be existing
Heater, for being preheated before entering the stage of reaction to material.
You need to add is that the size of each pipeline of gas-solid mixing device 10 provided in the embodiment of the present invention is unlimited, tool
Body needs are designed according to different technique, to meet different technique requirements.
Incorporated by reference to Fig. 2 and Fig. 4, the embodiment of the invention also provides a kind of gas-solid mixing system 20, including above-mentioned gas-solid are mixed
It attaches together and sets 10, can be reacted using superfine silicon slag, be uniformly mixed silicon slag with reaction gas, and then complete synthesis chlorine silicon
The reaction of alkane has good market application value.
Specifically, the reaction gas feed inlet 111 on mixed charge 110 can with the outlet of gas buffer tank, together
The import of sample injection pipe 120 is also with gas buffer tank outlet, and gas buffer tank is for storage reaction gas or indifferent gas
Body, wherein the charging nozzle of inert gas can be used for regulating gas flow velocity by flow control valve etc..In general, injection pipe
Gas flow rate in 120 reaches 300m/s or more and is advisable.
Specifically, solid material feed inlet 112 is connected to the outlet at bottom of the storage tank for storing silicon slag, the import of storage tank
It can be connected to other process stages, the silicon slag that other processes generate was conveyed as reaction raw materials.
Screw dust collector provided in an embodiment of the present invention (lower to be known as cooling exclusion device) is specifically described below.
Referring to figure 5., the embodiment of the invention provides a kind of cooling exclusion devices 40, including top cooler 130 and bottom
Slag device 140 is received in portion, and top cooler 130 is used to carry out gas cooling to deposit impurity, and slag device 140 is received for depositing in bottom
Put impurity solid.
Specifically, top cooler 130 includes cooling outer tube 131, the rotating mechanism 133 rotated in cooling outer tube 131
With the cooling collar 134 being arranged around cooling outer tube 131；Rotating mechanism 133 stretches in cooling outer tube 131, and rotating mechanism
It is formed between 133 and cooling outer tube 131 for the gas passage 132 for gas to be cooled circulation, the top of slag device 140 is received in bottom
Feed end is connected to gas passage 132；The cold liquid for cooling flow of media is formed between cooling collar 134 and cooling outer tube 131
Channel 135.
It should be noted that cooling exclusion device 40 provided in an embodiment of the present invention passes through in rotating mechanism 133 and cooling
It is passed through gas to be cooled between outer tube 131, is cooled down by the cooling collar 134 on cooling outer tube 131, is cooled down by regulation
Temperature deposits the impurity in gas, and by rotating mechanism 133 in cooling outer tube 131 rotation consolidating of making to deposit
Body falls to bottom and receives in slag device 140.Therefore, cooling exclusion device 40 provided in an embodiment of the present invention not only has cooling effect
Fruit, additionally it is possible to impurity is removed and collect, for cooling step can be passed through in the technical process using silicon slag synthesis chlorosilane
Metal chloride, such as copper chloride, alchlor, ferric trichloride, calcium chloride, magnesium chloride are removed, the purifying in later period is reduced
Journey, energy saving.
Further, rotating mechanism 133 includes rotation axis 1331 and the helical structure 1332 being fixed in rotation axis 1331,
The top of rotation axis 1331 is located at the top outer of cooling outer tube 131, and the bottom of rotation axis 1331 extends to cooling outer tube 131
Bottom, helical structure 1332 extend to the bottom of cooling outer tube 131 from the top of cooling outer tube 131.By driving rotation axis
1331 rotations drive the helical structure 1332 in rotation axis 1331 to rotate, fall into so that the impurity being deposited on tube wall be struck off
It receives in slag device 140 bottom of lower section.
Specifically, the tubular structure that helical structure 1332 can be arranged for general winding rotation axis 1331.In some realities
It applies in example, helical structure 1332 can be arranged in inner tube, make to form gas passage 132 between inner tube and cooling outer tube 131.
As it can be seen that the way of realization of helical structure 1332 is unlimited, be mainly that by will be deposited on during rotation it is miscellaneous on tube wall
Matter is struck off.
In order to more effectively strike off deposit, incorporated by reference to Fig. 5 and Fig. 6, helical structure 1332 is close to cooling 131 inner wall of outer tube
One end and cooling outer tube 131 inner wall between spacing be 0.3-5mm.Inventors have found that helical structure 1332 and cooling are outer
Deposit within the above range, can preferably be struck off and be collected by the spacing between pipe 131.
Further, rotating mechanism 133 further includes driving motor 1333, and driving motor 1333 is installed on cooling outer tube 131
Top, and the top of the output end of driving motor 1333 and rotation axis 1331 is sequentially connected, so that rotation axis 1331 drives spiral shell
Rotation structure 1332 rotates in cooling outer tube 131.Under the driving of driving motor 1333, rotation axis 1331 and helical structure 1332
It can rotate with it, can control revolving speed in actual moving process in 2-3r/mi n.
Specifically, driving motor 1333 is existing motor, and rotation axis 1331 can be driven to rotate under schedule speed.
In some embodiments, it can be not provided with driving motor 1333, but rotation is periodically driven by manually mode
Deposit is struck off in the rotation of axis 1331.
Specifically, the top of cooling collar 134 is provided with cooling medium outlet 1342, the bottom setting of cooling collar 134
There is cooling medium inlet 1344.Cooling medium is unlimited, can be the cooling water generallyd use, and cooling water is from cooling medium inlet
1344 be passed through after from 1342 output of cooling medium outlet, adjusted by regulating and controlling the temperature of cooling water being passed through in cooling collar 134
Control the cooling temperature of cooling exclusion device 40.
Further, cooling gas outlet 101 is located in the top sidewall of cooling outer tube 131, and cooling air import 102 is located at bottom
It receives on the side wall of slag device 140 in portion.In this way, gas to be cooled from cooling air import 102 entrance after upwardly through gas passage 132 after
It is exported from cooling gas outlet 101.
Further, the container with a narrow upper and lower width of slag device 140 is received in bottom, and the bottom of bottom receipts slag device 140 is provided with out
The form wide at the top and narrow at the bottom of slag device 140 is received convenient for discharging after collection material from slag notch 141 in cinder notch 141, bottom.
Further, it includes top section 142 and bottom stage 144 that slag device 140 is received in bottom, and top section 142 is cylindrical, bottom
In coniform, the bottom wall of top section 142 is fixedly connected section 144 with the roof of bottom stage 144.As shown in Figure 5, it strikes off
Metal chloride enters bottom stage 144 after passing through top section 142, and material can be discharged to cooling remove by opening slag notch 141
Miscellaneous device 40.
Fig. 7-Fig. 8 is please referred to, the embodiment of the invention also provides a kind of cooling systems 30, including 150 He of primary cooler
The cooling air import 102 of above-mentioned cooling exclusion device 40, the gas vent of primary cooler 150 and cooling exclusion device 40 connects
It is logical.Gas to be cooled enters back into the cooling removal of impurities of cooling exclusion device 40 after being cooled down by primary cooler 150, can be improved
The removal rate of impurity.
Further, primary cooler 150 includes cooling air inner tube 153 and the cooling medium outer tube for cooling flow of media
154, cooling medium outer tube 154 is arranged around cooling air inner tube 153, the outlet end of cooling air inner tube 153 and cooling exclusion device
40 cooling air import 102 is connected to.After gas to be cooled enters cooling air inner tube 153, by cold in cooling medium outer tube 154
But medium carry out it is cooling after, then entered in cooling exclusion device 40 by the outlet of cooling air inner tube 153 and cooled down again.
In general, the temperature of the cooling medium in primary cooler 150 is higher than cooling medium in cooling exclusion device 40
Temperature, actual temp needs set according to process requirement.
Specifically, the bottom of cooling medium outer tube 154 is provided with cooling medium inlet 151, the top of cooling medium outer tube 154
Portion is provided with cooling medium outlet 152.Cooling medium such as cooling water enters cooling medium outer tube 154 from cooling medium inlet 151
Behind gap between cooling air inner tube 153, the gas in cooling air inner tube 153 is cooled down, then can be situated between from cooling
152 output of matter outlet.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of methods using organosilicon silicon slag production chlorosilane, provide using the embodiment of the present invention
Gas-solid mixing device carry out silicon slag and reaction gas mixing, comprising the following steps:
Silicon slag feed inlet and reaction gas feed inlet are generated firstly, passing through using inert gas in mixing arrangement high speed
The negative pressure of 2kpa or so, and then it is uniformly mixed silicon slag and reaction gas in mixing arrangement, wherein the flow velocity of inert gas is
100m/s, reaction gas are hydrogen chloride, and the materials ratio of silicon slag and hydrogen chloride is 28:140.
Secondly, mixed gas is reacted under the conditions of about 240 DEG C of temperature, it is preliminary under the conditions of 130 DEG C or so of temperature
Cooling, then secondary cooling obtains chlorosilane gas under the conditions of 70 DEG C of temperature, will be deposited on cooling after secondary cooling process
Metal chloride in device is collected.
Finally, by the chlorosilane gas after secondary cooling under the conditions of 25 DEG C of temperature after cooling, using -20 DEG C of depth
It is cold to obtain product liquid；Product liquid is steamed into product liquid under the conditions of 100 DEG C of temperature, then in 25 DEG C of temperature condition
Deep cooling under the conditions of lower cooling, -20 DEG C of temperature eventually passes through rectifying separation.
Embodiment 2
The present embodiment provides a kind of methods using organosilicon silicon slag production chlorosilane, provide using the embodiment of the present invention
Gas-solid mixing device carry out silicon slag and reaction gas mixing, comprising the following steps:
Silicon slag feed inlet and reaction gas feed inlet are generated firstly, passing through using inert gas in mixing arrangement high speed
The negative pressure of 20kpa or so, and then it is uniformly mixed silicon slag and reaction gas in mixing arrangement, wherein the flow velocity of inert gas
For 300m/s, reaction gas is hydrogen chloride, and the materials ratio of silicon slag and hydrogen chloride is 56:140.
Secondly, mixed gas is reacted under the conditions of about 350 DEG C of temperature, it is preliminary under the conditions of 160 DEG C or so of temperature
Cooling, then secondary cooling obtains chlorosilane gas under the conditions of 130 DEG C of temperature, will be deposited on cooling after secondary cooling process
Metal chloride in device is collected.
Finally, by the chlorosilane gas after secondary cooling under the conditions of 35 DEG C of temperature after cooling, using -25 DEG C of depth
It is cold to obtain product liquid；Product liquid is steamed into product liquid under the conditions of 105 DEG C of temperature, then in 35 DEG C of temperature condition
Deep cooling under the conditions of lower cooling, -25 DEG C of temperature eventually passes through rectifying separation.
Embodiment 3
The present embodiment provides a kind of methods using organosilicon silicon slag production chlorosilane, provide using the embodiment of the present invention
Gas-solid mixing device carry out silicon slag and reaction gas mixing, comprising the following steps:
Silicon slag feed inlet and reaction gas feed inlet are generated firstly, passing through using inert gas in mixing arrangement high speed
The negative pressure of 15kpa or so, and then it is uniformly mixed silicon slag and reaction gas in mixing arrangement, wherein the flow velocity of inert gas
For 200m/s, reaction gas is chlorine, and the materials ratio of silicon slag and chlorine is 27:140.
Secondly, mixed gas is reacted under the conditions of about 300 DEG C of temperature, it is preliminary under the conditions of 150 DEG C or so of temperature
Cooling, then secondary cooling obtains chlorosilane gas under the conditions of 100 DEG C of temperature, will be deposited on cooling after secondary cooling process
Metal chloride in device is collected.
Finally, by the chlorosilane gas after secondary cooling under the conditions of 30 DEG C of temperature after cooling, using -23 DEG C of depth
It is cold to obtain product liquid；Product liquid is steamed into product liquid under the conditions of 103 DEG C of temperature, then in 30 DEG C of temperature condition
Deep cooling under the conditions of lower cooling, -23 DEG C of temperature eventually passes through rectifying separation.
Embodiment 4
The present embodiment provides a kind of method using organosilicon silicon slag production chlorosilane, specific steps and embodiment 3 are big
It causes identical, the difference is that only that the materials ratio of silicon slag and chlorine is 55:140.
Comparative example 1
This comparative example provides a kind of method using organosilicon silicon slag production chlorosilane, and specific steps and embodiment 1 are big
Cause it is identical, the difference is that silicon slag and reaction gas are to be mixed by way of conventional, rather than apply above-mentioned gas-solid
Mixing arrangement.
Test example 1
The utilization rate of silicon slag in testing example 1-4 and comparative example 1, test method: silicon slag is added in metering star feeder
The liquid level h of 1 gained chlorosilane of mass M converse volume V, by silicon tetrachloride relative density 1480kg/m3, can convert and produce
The amount M2 of product passes through formula by trichlorosilane relative density 1350kg/m3, the amount M3 that can be converted into product: utilization rate=
(M2/170+M3/135.5) * 28/M1*100%.
Silicon slag utilization rate is respectively as follows: 95%, 92%, 86%, 91%, 20% in embodiment 1-4 and comparative example 1.Thus may be used
See, mixing method provided in an embodiment of the present invention can make full use of silicon slag, and silicon slag utilization rate is truly realized 85% or more
The efficient utilization of silicon slag has good market application value.
Test example 2
It is as a result as follows using the purity of conventional method test chlorosilane product:
Contain 87% trichlorosilane, about 10% silicon tetrachloride in embodiment 1 before rectifying；Product purity reaches after rectifying
To 99%.
The product purity of silicon tetrachloride is 97% before rectifying in embodiment 3, and product purity is 99% after rectifying.
In conclusion a kind of beneficial effect of method using organosilicon silicon slag production chlorosilane provided by the invention is:
It makes silicon slag and reaction gas by generating negative pressure in silicon slag feed inlet and reaction gas feed inlet in the current inert gas of height
Body is uniformly mixed in mixing arrangement；Silicon slag and reaction gas reaction production chlorosilane, regulate and control cooling temperature by step cooling
So that metal chloride is deposited removal in secondary cooling, obtain more pure chlorosilane gas, the utilization rate of silicon slag exists
85% or more, realization is turned waste into wealth.
A kind of device using organosilicon silicon slag production chlorosilane provided in an embodiment of the present invention, for above-mentioned using organic
The method that silicon silicon slag produces chlorosilane realizes being sufficiently mixed for silicon slag and reaction gas by improving gas-solid mixing device, into
And by obtaining chlorosilane product after reaction and removal of impurities.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of method using organosilicon silicon slag production chlorosilane, which comprises the steps of:
Keep gas current in mixing arrangement high speed in the way of injection inert gas or reaction gas, make silicon slag feed inlet and
Reaction gas feed inlet generates negative pressure, and then is uniformly mixed the silicon slag and the reaction gas in the mixing arrangement,
Wherein, the inert gas or the flow velocity of reaction gas injection are 100-300m/s, and the reaction gas is hydrogen chloride or chlorine；
Mixed gas is reacted under the conditions of 240-350 DEG C of temperature, is obtained then in turn through preliminary cooling and secondary cooling
Chlorosilane gas, wherein the temperature of gas controls the gas temperature control after 130-160 DEG C, secondary cooling and exists after preliminary cooling
70-130℃。
2. the method according to claim 1 using organosilicon silicon slag production chlorosilane, which is characterized in that fed in silicon slag
The negative pressure that mouth and reaction gas feed inlet generate is 2-20kpa；
Preferably, if injection gas is inert gas, the injection flow of inert gas is 20-30m3/ h connects at slag charge feed inlet
The revolving speed of the batcher connect is 10-15r/min；
If injection gas is reaction gas, the injection flow of reaction gas is 15-25m3/ h, what is connected at slag charge feed inlet gives
The revolving speed of material machine is 8-12r/min.
3. the method according to claim 1 using organosilicon silicon slag production chlorosilane, which is characterized in that the reaction gas
When body is hydrogen chloride, the weight ratio of the silicon slag and the reaction gas is 50:150-200.
4. the method according to claim 1 using organosilicon silicon slag production chlorosilane, which is characterized in that the reaction gas
When body is chlorine, the weight ratio of the silicon slag and the reaction gas is 50:230-300.
5. the method according to claim 1 using organosilicon silicon slag production chlorosilane, which is characterized in that described secondary
The metal chloride being deposited in cooler is collected after cooling procedure.
6. the method according to claim 1 using organosilicon silicon slag production chlorosilane, which is characterized in that the utilization has
The method of machine silicon silicon slag production chlorosilane further includes that the chlorosilane gas after secondary cooling is obtained four chlorinations by multistage cooling
Silicon or trichlorosilane liquid product.
7. the method according to claim 6 using organosilicon silicon slag production chlorosilane, which is characterized in that the multistage is cold
But after process includes the chlorosilane gas is cooling under the conditions of 25-35 DEG C of temperature, using -20~-25 DEG C of deep cooling.
8. the method according to claim 6 using organosilicon silicon slag production chlorosilane, which is characterized in that the utilization has
The method of machine silicon silicon slag production chlorosilane further include will it is multistage cooling after the temperature condition of obtained product liquid at 100-105 DEG C
Under steam product liquid, the then deep cooling under the conditions of cooling, -20~-25 DEG C of temperature under the conditions of 25-35 DEG C of temperature, finally
It is separated by rectifying.
9. a kind of device using organosilicon silicon slag production chlorosilane, for implementing utilization described in any one of claim 1-8
The method of organosilicon silicon slag production chlorosilane, which is characterized in that including raw material conveying device, the gas-solid mixing dress set gradually
It sets, heating response device, primary cooler, secondary coolers and product purifying device；
The raw material conveying device includes inert gas delivery pipe and reaction letter shoot；
The gas-solid mixing device includes the injection pipe that mixed charge and caliber are less than the mixed charge, and the one of the injection pipe
End is located at outside the mixed charge, and the other end of the injection pipe stretches in the mixed charge；
Reaction gas feed inlet and solid material feed inlet are provided on the mixed charge, the inert gas delivery pipe goes out
The outlet of the inlet communication of mouth and the injection pipe, the reaction letter shoot is connected to the reaction gas feed inlet.
10. the device according to claim 9 using organosilicon silicon slag production chlorosilane, which is characterized in that the mixing
Supervisor includes segmental arc and mixing section, and the reaction gas feed inlet is located at the top of the segmental arc, the bottom of the segmental arc
Portion is connected with one end of the mixing section, and described injection pipe one end is located at the outside of the segmental arc, and the other end is from the arc
Shape section protrudes into the mixed charge and extends to the mixing section；
The mixing section includes the first mixing section and the second mixing section, the bottom of the segmental arc and the one of first mixing section
End is connected, the inlet communication of the other end of first mixing section and second mixing section；
The caliber of second mixing section is less than the caliber of first mixing section, and the caliber of second mixing section is greater than institute
State the caliber of injection pipe.
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| CN201811333009.9A CN109292781B (en) | 2018-11-09 | 2018-11-09 | Method and device for producing chlorosilane by using organosilicon silicon slag |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4224297A (en) * | 1977-07-22 | 1980-09-23 | Wacker-Chemie Gmbh | Method for reactivating a residue containing elemental silicon |
| CN204823256U (en) * | 2015-07-08 | 2015-12-02 | 陕西延长石油（集团）有限责任公司 | Carbon containing solid material's mixed dispenser |
| CN108069428A (en) * | 2016-11-18 | 2018-05-25 | 江苏中能硅业科技发展有限公司 | For handling the device and technique of polysilicon by-product slurry |
-
2018
- 2018-11-09 CN CN201811333009.9A patent/CN109292781B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4224297A (en) * | 1977-07-22 | 1980-09-23 | Wacker-Chemie Gmbh | Method for reactivating a residue containing elemental silicon |
| CN204823256U (en) * | 2015-07-08 | 2015-12-02 | 陕西延长石油（集团）有限责任公司 | Carbon containing solid material's mixed dispenser |
| CN108069428A (en) * | 2016-11-18 | 2018-05-25 | 江苏中能硅业科技发展有限公司 | For handling the device and technique of polysilicon by-product slurry |
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Effective date of registration: 20240318 Address after: 610000 Xincai 18th Road, new material industrial functional zone, Xinjin Industrial Park, Xinjin County, Chengdu City, Sichuan Province Patentee after: CHENGDU SHULING TECHNOLOGY DEVELOPMENT Co.,Ltd. Country or region after: China Address before: 611400 No. 445, Qingyun South Road, Puxing street, Xinjin District, Xinjin County, Chengdu, Sichuan Patentee before: Sichuan mintian Technology Development Co.,Ltd. Country or region before: China |