CN112408396A - A kind of process and equipment for removing aluminum by chlorosilane complexation - Google Patents
A kind of process and equipment for removing aluminum by chlorosilane complexation Download PDFInfo
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- CN112408396A CN112408396A CN202011378676.6A CN202011378676A CN112408396A CN 112408396 A CN112408396 A CN 112408396A CN 202011378676 A CN202011378676 A CN 202011378676A CN 112408396 A CN112408396 A CN 112408396A
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 456
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 455
- 239000005046 Chlorosilane Substances 0.000 title claims abstract description 271
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 title claims abstract description 271
- 238000000034 method Methods 0.000 title claims abstract description 105
- 230000008569 process Effects 0.000 title claims abstract description 92
- 238000010668 complexation reaction Methods 0.000 title claims abstract description 14
- 230000000536 complexating effect Effects 0.000 claims abstract description 389
- 239000002994 raw material Substances 0.000 claims abstract description 225
- 238000003756 stirring Methods 0.000 claims abstract description 214
- 239000007791 liquid phase Substances 0.000 claims abstract description 192
- 239000012071 phase Substances 0.000 claims abstract description 151
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 108
- 239000000203 mixture Substances 0.000 claims abstract description 99
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 52
- 239000007789 gas Substances 0.000 claims description 119
- 239000000047 product Substances 0.000 claims description 111
- 239000007788 liquid Substances 0.000 claims description 59
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 50
- 238000001704 evaporation Methods 0.000 claims description 42
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 35
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 34
- 230000008020 evaporation Effects 0.000 claims description 31
- 239000011863 silicon-based powder Substances 0.000 claims description 31
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 30
- 239000012535 impurity Substances 0.000 claims description 29
- 239000002893 slag Substances 0.000 claims description 29
- 238000010438 heat treatment Methods 0.000 claims description 28
- 235000011164 potassium chloride Nutrition 0.000 claims description 25
- 239000001103 potassium chloride Substances 0.000 claims description 25
- 239000012263 liquid product Substances 0.000 claims description 20
- 238000011049 filling Methods 0.000 claims description 18
- 239000002699 waste material Substances 0.000 claims description 16
- -1 alkaline earth metal salt Chemical class 0.000 claims description 15
- 239000011780 sodium chloride Substances 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 238000012546 transfer Methods 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 11
- 238000005086 pumping Methods 0.000 claims description 10
- 239000011148 porous material Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 229910052698 phosphorus Inorganic materials 0.000 claims description 7
- 239000002879 Lewis base Substances 0.000 claims description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- 229910052783 alkali metal Inorganic materials 0.000 claims description 6
- 150000001340 alkali metals Chemical class 0.000 claims description 6
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 150000007527 lewis bases Chemical class 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 238000012856 packing Methods 0.000 claims description 6
- 239000011574 phosphorus Substances 0.000 claims description 6
- 229910052717 sulfur Inorganic materials 0.000 claims description 6
- 239000011593 sulfur Substances 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 238000001179 sorption measurement Methods 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 2
- 208000028659 discharge Diseases 0.000 description 42
- XHFGWHUWQXTGAT-UHFFFAOYSA-N dimethylamine hydrochloride Natural products CNC(C)C XHFGWHUWQXTGAT-UHFFFAOYSA-N 0.000 description 14
- IQDGSYLLQPDQDV-UHFFFAOYSA-N dimethylazanium;chloride Chemical compound Cl.CNC IQDGSYLLQPDQDV-UHFFFAOYSA-N 0.000 description 14
- 238000001035 drying Methods 0.000 description 14
- 238000005984 hydrogenation reaction Methods 0.000 description 11
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000002156 mixing Methods 0.000 description 5
- 229920005591 polysilicon Polymers 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000007792 gaseous phase Substances 0.000 description 3
- 229910001510 metal chloride Inorganic materials 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 150000001282 organosilanes Chemical class 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 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 1
- 235000011299 Brassica oleracea var botrytis Nutrition 0.000 description 1
- 240000003259 Brassica oleracea var. botrytis Species 0.000 description 1
- 235000014653 Carica parviflora Nutrition 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000243321 Cnidaria Species 0.000 description 1
- 102000015833 Cystatin Human genes 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- FPCDPCXGRZRIQK-UHFFFAOYSA-N [Si]([O-])([O-])([O-])Cl.[Al+3] Chemical compound [Si]([O-])([O-])([O-])Cl.[Al+3] FPCDPCXGRZRIQK-UHFFFAOYSA-N 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 108050004038 cystatin Proteins 0.000 description 1
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 150000001367 organochlorosilanes Chemical class 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
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
- C01B33/10778—Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
本发明涉及一种氯硅烷络合除铝的工艺及装备；对低温络合除铝工艺、液相络合除铝工艺、气相络合工艺和高压精馏除铝工艺单独或组合操作来满足不同的氯硅烷提纯要求。低温络合搅拌罐过滤器过滤后的氯硅烷混合物和原料缓冲罐输送的原料经过低温络合除铝进出换热器进行换热，实现能量的有效利用。低温络合除铝剂、液相除铝剂和气相除铝剂的使用寿命较长，络合除铝效果明显。本发明可供选择使用的络合除铝剂种类较多，在工艺操作范围条件下能保持较高的络合除铝的性能。提高氯硅烷的铝脱除率，通过低温络合除铝和液相络合除铝工艺将氯硅烷中氯化铝含量降低，最后通过串联气相络合除铝和高压精馏除铝工艺可使氯硅烷中铝含量降低至0.001ppm以下。
The invention relates to a process and equipment for chlorosilane complex aluminum removal; the low temperature complex aluminum removal process, the liquid phase complex aluminum removal process, the gas phase complexation process and the high-pressure rectification aluminum removal process can be operated individually or in combination to meet different requirements. chlorosilane purification requirements. The chlorosilane mixture filtered by the low-temperature complexing stirring tank filter and the raw materials transported by the raw material buffer tank pass through the low-temperature complexing and aluminum removal into and out of the heat exchanger for heat exchange to realize the effective utilization of energy. The low temperature complex aluminum remover, the liquid phase aluminum remover and the gas phase aluminum remover have a long service life, and the complex aluminum remover has an obvious effect. There are many kinds of complex aluminum removing agents that can be selected and used in the present invention, and can maintain high complex aluminum removing performance under the conditions of technological operation range. To improve the aluminum removal rate of chlorosilane, the aluminum chloride content in chlorosilane is reduced by the low temperature complex aluminum removal and liquid phase complex aluminum removal process, and finally the series gas phase complex aluminum removal and high pressure rectification aluminum removal process can make the aluminum chloride removal process. The aluminum content in the chlorosilane was reduced to below 0.001 ppm.
Description
Technical Field
The invention relates to the technical field of complexing impurity removal, in particular to a process and equipment for removing aluminum and purifying chlorosilane by utilizing low-temperature complexing and liquid-phase complexing in a polycrystalline silicon production process. In particular to a process and equipment for removing aluminum by chlorosilane complexation.
Background
Chlorosilanes are used in the synthesis of organosilanes and alkyl, aryl and organofunctional chlorosilanes and are the most basic monomers in organosilane coupling agents and also raw materials for the production of semiconductor silicon, single crystal silicon and polycrystalline silicon.
In many processes for producing high-purity silicon, liquid chlorosilanes are first produced industrially from metallurgical-grade silicon powder having a purity of about 99%, which chlorosilanes can be purified to very high purity and then converted back into very high-purity solid crystalline silicon. In the organosilicon industry, high purity organochlorosilanes are also used in the preparation of organosilicon monomers and downstream products.
The impurities contained in the industrial grade silicon powder used as the raw material for production are one of the main sources of the impurities in the production process of the polycrystalline silicon. At present, primary polysilicon is mainly produced by an improved Siemens method, and is divided into coral material, cauliflower material, carbon head material and the like according to different qualities and appearances, and the purity of silicon is approximately 99.9999%. With the exception of P, B in the native polysilicon. Mainly contains non-metallic impurities such as O, C and metallic impurities such as Fe and Al.
In the production process of polycrystalline silicon, the discharged chlorosilane of the cold hydrogenation system contains aluminum-containing impurities, and is discharged as waste through hydrolysis treatment in the past, so that a large amount of water resources are consumed, and the environment is polluted. In order to recycle chlorosilane, aluminum removal operation on cold hydrogenation slag discharge is required, and rectification removal is usually adopted, but the effect is general.
During the reaction, the reactor generally has the following conditions: the impurity-containing silicon powder reacts with the chlorine-containing gas, and many solid impurities remain in the reactor or in a dust removing device such as a cyclone. However, since aluminum-containing impurities, especially chloride impurities, are extremely sublimable due to their chemical nature and can form volatile compounds which are carried out of the reactor with the desired chlorosilane starting material, chlorosilanes are produced which contain aluminum-containing chloride impurities in amounts which are high, usually in the form of aluminum impuritiesAluminium chloride (AlCl)3). The effluent gas from the reactor thus contains volatile compounds of aluminum chloride, and the effluent gas is subsequently cooled to form a liquid chlorosilane mixture which can be purified by conventional methods, primarily by distillation. If aluminum removal operation is not carried out, the subsequent production process is influenced by the existence of aluminum chloride impurities, so that the quality of polycrystalline silicon or organic silicon products is influenced. In metallurgical grade silicon powder feedstock, aluminum is the major impurity, about 2000-10000ppm, so the aluminum content must be reduced to very low levels. Furthermore, aluminium chloride (AlCl)3) Having the unusual property that no liquid phase is formed at atmospheric pressure, aluminum chloride can sublime directly from solid to gas when the pressure is close to atmospheric pressure, such as for distillation. Therefore, it is very difficult to remove aluminum chloride by distillation, and a major disadvantage of the existing distillation separation technology is that aluminum chloride sublimates in a gas phase under normal conditions and diffuses into the whole column, so that aluminum in the whole column cannot be separated, and aluminum chloride in a solid state cannot be deposited, and finally only the operation of the column can be stopped for cleaning, so that a special method and a special device are needed for effectively performing the rectification process.
Most of the prior patents relating to the preparation of chlorosilanes do not mention the removal of metal chlorides nor the removal of aluminum chloride impurities from chlorosilanes by low temperature complexation. In the chinese utility model patent No. CN 210825446U "zero discharge treatment system for cold hydrogenation of slag slurry", only the relevant flow of the slag slurry treatment system is mentioned. After liquid chlorosilane containing silicon powder from a cold hydrogenation device is treated by a slurry system, the silicon powder and the chlorosilane are recovered and reused in a polysilicon production system, and relevant processes and equipment for removing aluminum-containing chloride are not described.
In the invention patent No. CN 101925532a of stefin M old, "method for removing aluminum and other metal chlorides from chlorosilanes", only the introduction of a seed crystal source into an impure liquid chlorosilane source and the separation after the crystallization of aluminum and other metal chlorides on the seed crystals in the liquid chlorosilanes in a stirred vessel are described, but there is no explicit description of the aluminum removal by low-temperature complexation, liquid-phase complexation and gas-phase complexation, and there is no description of other complex aluminum removal processes and apparatuses.
The problem of aluminum impurity treatment in chlorosilane is gradually a difficult problem which troubles some polysilicon production enterprises in China. At present, no process and equipment for removing aluminum from chlorosilane are introduced at home and abroad. The invention removes aluminum by low-temperature complexing, further reduces the content of aluminum chloride in the chlorosilane by combining liquid phase and gas phase complexing processes, and finally obtains the chlorosilane almost free of aluminum by a high-pressure rectification process. The complex is generated through the complex reaction of the aluminum removing agent and aluminum chloride, so that the aluminum impurities in the slag-off chlorosilane of a cold hydrogenation system are removed, the chlorosilane raw material is recycled, and the raw material utilization rate is improved.
Disclosure of Invention
The invention mainly aims to provide a process and equipment for removing aluminum by chlorosilane complexation, which are used for removing aluminum chloride serving as an impurity of a waste chlorosilane mixture subjected to cold hydrogenation slag removal in the production process of an improved Siemens method to obtain a high-purity chlorosilane raw material almost free of aluminum for recycling to prepare a high-purity polysilicon or organosilicon product.
The invention relates to a complex reaction which mainly comprises the following steps: (CH)3)2NH·HCl+AlCl3→(CH3)2NH2Cl·AlCl3；AlCl3+LiCl→LiCl·AlCl3；AlCl3+NaCl→NaCl·AlCl3；AlCl3+KCl→KCl·AlCl3。
The process for removing aluminum by complexing chlorosilane disclosed by the invention utilizes low temperature to remove aluminum by complexing, combines a liquid phase complexing aluminum removal process, can greatly reduce the content of aluminum impurities in chlorosilane, and can finally obtain the chlorosilane almost free of aluminum by serially connecting a gas phase complexing aluminum removal process and a high-pressure rectification process.
The invention relates to equipment for removing aluminum by complexing chlorosilane, which is characterized by comprising the following components: the system comprises a stirring settling tank, a dryer, a stirring settling tank filter, a raw material condenser, a raw material buffer tank, a raw material delivery pump, a low-temperature complexing and aluminum-removing inlet and outlet heat exchanger, a low-temperature cooler, a low-temperature complexing and stirring tank filter, a low-temperature complexing and delivery pump, a liquid-phase aluminum-removing preheater, a liquid-phase aluminum-removing tank, a product buffer tank and a product discharge pump; wherein the bottom of the stirring and settling tank is connected with a dryer, and the lateral line of the stirring and settling tank is connected with a stirring and settling tank filter; the upper part of the dryer is connected with a raw material condenser; the bottom of the stirring and settling tank filter and the outlet of the raw material condenser are connected with a raw material buffer tank; the raw material delivery pump at the bottom of the raw material buffer tank is connected with a feed inlet of the low-temperature complexing aluminum-removing inlet-outlet heat exchanger; the low-temperature complexing and aluminum removing inlet and outlet heat exchanger feed outlet is connected with the low-temperature cooler inlet; the outlet of the low-temperature cooler is connected with the top of the low-temperature complexing stirring tank; the low-temperature complexing transfer pump at the bottom of the low-temperature complexing stirring tank is connected with a low-temperature complexing stirring tank filter; the bottom of the low-temperature complexing stirring tank filter is connected with a dryer, and the lateral line of the low-temperature complexing and aluminum-removing filter is connected with a discharge inlet of the low-temperature complexing heat exchanger; the outlet of the low-temperature complexing aluminum removal inlet-outlet heat exchanger is connected with the inlet of the liquid-phase aluminum removal preheater; the outlet of the liquid-phase aluminum removal preheater is connected with a liquid-phase aluminum removal tank; the top of the product buffer tank is connected with a liquid phase aluminum removal tank, and the bottom of the product buffer tank is connected with a product discharge pump; and pumping out the chlorosilane product after the aluminum is removed by a product discharge pump.
The invention relates to a process for removing aluminum by chlorosilane complexation, which comprises the steps of feeding a chlorosilane mixture containing aluminum impurities at the top of a stirring settling tank, settling and separating, drying and separating silicon powder and aluminum slag from a tank bottom mixture by a dryer, and condensing the mixture into a raw material buffer tank by a raw material condenser; the chlorosilane mixture extracted from the side line enters a raw material buffer tank after being filtered and separated by a stirring settling tank filter; the method comprises the following steps of pre-cooling raw materials in a low-temperature complexing and dealuminizing inlet and outlet heat exchanger through low-temperature complexing dealuminizing, cooling the raw materials through a low-temperature cooler, removing aluminum in a low-temperature complexing stirring tank filled with a low-temperature complexing dealuminizing agent, filtering the raw materials through a low-temperature complexing stirring tank filter to remove aluminum chloride waste residues, exchanging heat between a chlorosilane mixture filtered by the low-temperature complexing stirring tank filter and the raw materials conveyed by a raw material buffer tank through the low-temperature complexing dealuminizing inlet and; heating chlorosilane through a liquid-phase dealuminization preheater, and feeding the heated chlorosilane into a liquid-phase dealuminization tank filled with a liquid-phase dealuminization agent for dealuminization; liquid chlorosilane subjected to liquid phase aluminum removal enters a product buffer tank and is transported out through a product discharge pump; and removing aluminum from the chlorosilane mixture through low-temperature complexing and liquid-phase complexing to obtain a high-purity chlorosilane liquid product almost free of aluminum.
The low-temperature complexing aluminum-removing inlet-outlet heat exchanger precools the raw materials to-10-0 ℃; the low-temperature cooler cools the chlorosilane to a temperature range of-20 ℃ to-30 ℃.
The liquid-phase aluminum removal preheater preheats the chlorosilane mixture subjected to low-temperature complexing aluminum removal to 20-30 ℃.
The low-temperature complexing aluminum remover and the liquid-phase aluminum remover adopt alkali metal, alkaline earth metal salt or a compound thereof, Lewis base containing nitrogen, oxygen, sulfur and phosphorus or a compound thereof, or a mixture of the above substances, preferably lithium chloride, sodium chloride, potassium chloride and amine compounds.
The filling amount of the low-temperature complexing aluminum remover and the liquid-phase aluminum remover is 40-50% of the volume of the tank.
The aluminum impurities are mainly aluminum chloride impurities.
The chlorosilane is silane, dichlorosilane, trichlorosilane, silicon tetrachloride, monochlorotrihydrogensilicon, organic chlorosilane or a mixture of the substances obtained by cold hydrogenation and deslagging.
In order to improve the aluminum removal rate of the chlorosilane, the aluminum chloride content in the chlorosilane can be reduced to 0.01ppm-0.1ppm by low-temperature complexing aluminum removal and liquid-phase complexing aluminum removal processes.
The equipment for removing aluminum by complexing chlorosilane is characterized by also being capable of being combined with a gas phase complexing aluminum removal process or a high-pressure rectification aluminum removal process in series for removing aluminum by chlorosilane.
When the gas phase complexing aluminum removal process is connected in series, the added equipment comprises: an evaporation kettle, a gas phase heater, a gas phase aluminum removal column and a gas phase condenser; wherein the bottom of the stirring and settling tank is connected with a dryer, and the lateral line of the stirring and settling tank is connected with a stirring and settling tank filter; the upper part of the dryer is connected with a raw material condenser; the stirring settling tank filter and the raw material condenser are connected with the raw material buffer tank; the raw material delivery pump at the bottom of the raw material buffer tank is connected with a feed inlet of the low-temperature complexing aluminum-removing inlet-outlet heat exchanger; the low-temperature complexing and aluminum removing inlet and outlet heat exchanger feed outlet is connected with the low-temperature cooler inlet; the outlet of the low-temperature cooler is connected with the top of the low-temperature complexing stirring tank; the low-temperature complexing transfer pump at the bottom of the low-temperature complexing stirring tank is connected with a low-temperature complexing stirring tank filter; the bottom of the low-temperature complexing stirring tank filter is connected with a dryer, and the lateral line of the low-temperature complexing and aluminum-removing filter is connected with a discharge inlet of the low-temperature complexing heat exchanger; the outlet of the low-temperature complexing aluminum removal inlet-outlet heat exchanger is connected with the inlet of the liquid-phase aluminum removal preheater; the outlet of the liquid-phase aluminum removal preheater is connected with a liquid-phase aluminum removal tank; at the moment, the bottom of the liquid phase aluminum removal tank is connected with an evaporation kettle; the evaporation kettle is connected with the inlet of the gas phase heater; the outlet of the gas phase heater is connected with the bottom of the gas phase aluminum removal column; the top of the gas phase aluminum removal column is connected with the inlet of a gas phase condenser; the outlet of the gas phase condenser is connected with a product buffer tank; and the chlorosilane products in the tank are pumped out by a product discharge pump and transported outside.
In the corresponding process after the serial gas-phase complexing aluminum removal, a chlorosilane mixture containing aluminum impurities is fed at the top of a stirring settling tank, is subjected to settling separation, and a tank bottom mixture is dried by a dryer to separate silicon powder and aluminum slag, and then is condensed by a raw material condenser to enter a raw material buffer tank; the chlorosilane mixture extracted from the side line enters a raw material buffer tank after being filtered and separated by a stirring settling tank filter; the method comprises the following steps of pre-cooling raw materials in a low-temperature complexing and dealuminizing inlet and outlet heat exchanger through low-temperature complexing dealuminizing, cooling the raw materials through a low-temperature cooler, removing aluminum in a low-temperature complexing stirring tank filled with a low-temperature complexing dealuminizing agent, filtering the raw materials through a low-temperature complexing stirring tank filter to remove aluminum chloride waste residues, exchanging heat between a chlorosilane mixture filtered by the low-temperature complexing stirring tank filter and the raw materials conveyed by a raw material buffer tank through the low-temperature complexing dealuminizing inlet and; heating chlorosilane through a liquid-phase dealuminization preheater, and feeding the heated chlorosilane into a liquid-phase dealuminization tank filled with a liquid-phase dealuminization agent for dealuminization; evaporating and gasifying liquid chlorosilane subjected to liquid phase dealuminization through an evaporation kettle, heating the liquid chlorosilane through a gas phase heater, introducing the liquid chlorosilane into a gas phase dealuminization column filled with a gas phase complexing dealuminization agent for dealuminization, condensing the gas phase chlorosilane from the top of the gas phase dealuminization column to be in a liquid state through a gas phase condenser, and transporting the liquid chlorosilane to a product buffer tank through a product discharge pump; and (3) performing low-temperature complexing and liquid-phase complexing aluminum removal on the chlorosilane mixture, and performing serial gas-phase complexing aluminum removal on the chlorosilane mixture to obtain a high-purity chlorosilane liquid product almost free of aluminum.
The gas-phase heater heats chlorosilane mixed steam from the evaporation kettle to 120-140 ℃.
The gas phase aluminum remover adopts alkali metal, alkaline earth metal salt or a compound thereof loaded by a porous material, and Lewis base containing nitrogen, oxygen, sulfur and phosphorus or a compound thereof loaded by the porous material, preferably lithium chloride, sodium chloride, potassium chloride and amine compounds loaded by the porous material.
The filling height of the gas phase aluminum remover is 70-80% of the height of the adsorption column. Wherein, the gas phase aluminum remover carrier is active carbon or active alumina material with porous structure, and the loading amount is 5-15% of the carrier mass.
In order to improve the aluminum removal rate of the chlorosilane, the aluminum chloride content in the chlorosilane can be reduced to 0.001ppm-0.01ppm by connecting a low-temperature complexing aluminum removal process and a liquid-phase complexing aluminum removal process in series with a gas-phase complexing aluminum removal process.
When the aluminum removing process is carried out by high-pressure rectification in series, the added equipment comprises: a high-pressure rectifying tower preheater and a high-pressure rectifying tower; a high-pressure rectifying tower condenser and a high-pressure rectifying tower evaporator; wherein the bottom of the stirring and settling tank is connected with a dryer, and the lateral line of the stirring and settling tank is connected with a stirring and settling tank filter; the upper part of the dryer is connected with a raw material condenser; the stirring settling tank filter and the raw material condenser are connected with the raw material buffer tank; the raw material delivery pump at the bottom of the raw material buffer tank is connected with a feed inlet of the low-temperature complexing aluminum-removing inlet-outlet heat exchanger; the low-temperature complexing and aluminum removing inlet and outlet heat exchanger feed outlet is connected with the low-temperature cooler inlet; the outlet of the low-temperature cooler is connected with the top of the low-temperature complexing stirring tank; the low-temperature complexing transfer pump at the bottom of the low-temperature complexing stirring tank is connected with a low-temperature complexing stirring tank filter; the bottom of the low-temperature complexing stirring tank filter is connected with a dryer, and the lateral line of the low-temperature complexing and aluminum-removing filter is connected with a discharge inlet of the low-temperature complexing heat exchanger; the outlet of the low-temperature complexing aluminum removal inlet-outlet heat exchanger is connected with the inlet of the liquid-phase aluminum removal preheater; the outlet of the liquid-phase aluminum removal preheater is connected with a liquid-phase aluminum removal tank; the top of the product buffer tank is connected with a liquid phase aluminum removal tank, and the bottom of the product buffer tank is connected with a product discharge pump; at the moment, the product discharge pump is connected with the inlet of a high-pressure rectifying tower preheater; the outlet of the high-pressure rectifying tower preheater is connected with the middle feeding position of the high-pressure rectifying tower; the high-pressure rectifying tower is provided with a tower top condenser and a tower bottom evaporator.
In the corresponding process after the aluminum is removed by the series high-pressure rectification, a chlorosilane mixture containing aluminum impurities is fed at the top of a stirring settling tank, is subjected to settling separation, and a tank bottom mixture is dried by a dryer to separate silicon powder and aluminum slag, and then is condensed by a raw material condenser to enter a raw material buffer tank; the chlorosilane mixture extracted from the side line enters a raw material buffer tank after being filtered and separated by a stirring settling tank filter; the method comprises the following steps of pre-cooling raw materials in a low-temperature complexing and dealuminizing inlet and outlet heat exchanger through low-temperature complexing dealuminizing, cooling the raw materials through a low-temperature cooler, removing aluminum in a low-temperature complexing stirring tank filled with a low-temperature complexing dealuminizing agent, filtering the raw materials through a low-temperature complexing stirring tank filter to remove aluminum chloride waste residues, exchanging heat between a chlorosilane mixture filtered by the low-temperature complexing stirring tank filter and the raw materials conveyed by a raw material buffer tank through the low-temperature complexing dealuminizing inlet and; heating chlorosilane through a liquid-phase dealuminization preheater, and feeding the heated chlorosilane into a liquid-phase dealuminization tank filled with a liquid-phase dealuminization agent for dealuminization; liquid chlorosilane subjected to liquid phase dealuminization is conveyed to a product buffer tank, chlorosilane in the tank is conveyed to a high-pressure rectifying tower preheater through a product discharge pump and heated, then the liquid chlorosilane is introduced into a high-pressure rectifying tower for high-pressure rectifying dealuminization, finally, an aluminum-containing high-boiling-point substance is separated from the bottom of an evaporator of the high-pressure rectifying tower, and after the purified chlorosilane is condensed and liquefied by a condenser of the high-pressure rectifying tower, part of the purified chlorosilane is extracted to obtain a high-purity chlorosilane liquid product subjected to dealuminization. And (3) performing low-temperature complexing and liquid-phase complexing aluminum removal on the chlorosilane mixture, and performing high-pressure rectification aluminum removal on the chlorosilane mixture to obtain a high-purity chlorosilane liquid product almost free of aluminum.
The upper section and the lower section in the high-pressure rectifying tower are random packing or regular packing.
The high-pressure rectifying tower is provided with partial reflux at the top of the tower through a condenser.
The high-pressure rectifying tower preheater preheats chlorosilane to 180-220 ℃; and the operating pressure of the high-pressure rectifying tower is controlled to be 15-35 atm.
In order to improve the aluminum removal rate of the chlorosilane, the aluminum chloride content in the chlorosilane can be reduced to 0.001ppm-0.01ppm by connecting a low-temperature complexing aluminum removal process and a liquid-phase complexing aluminum removal process in series with a high-pressure rectification aluminum removal process.
The complexing aluminum-removing process can be simultaneously connected in series with a gas-phase complexing aluminum-removing process and a high-pressure rectifying aluminum-removing process, and the gas-phase complexing aluminum-removing process is firstly connected in series and then connected in series with the high-pressure rectifying aluminum-removing process for continuous aluminum-removing operation, so that the content of aluminum chloride can be reduced to be below 0.001 ppm.
When the gas phase complexing aluminum removal and high-pressure rectification aluminum removal processes are connected in series, the equipment comprises: stirring settling cask, the desiccator, stirring settling cask filter, raw materials condenser, the raw materials buffer tank, the raw materials delivery pump, low temperature complex removes aluminium business turn over heat exchanger, the cryocooler, low temperature complex agitator tank filter, low temperature complex delivery pump, liquid phase removes aluminium pre-heater, liquid phase removes aluminium jar, the evaporation kettle, the gaseous phase heater, gaseous phase removes aluminium post, the gaseous phase condenser, the product buffer tank, the product discharge pump, high-pressure rectifying column pre-heater, high-pressure rectifying column condenser, high-pressure rectifying column evaporimeter.
Wherein the bottom of the stirring and settling tank is connected with a dryer, and the lateral line of the stirring and settling tank is connected with a stirring and settling tank filter; the upper part of the dryer is connected with a raw material condenser; the stirring settling tank filter and the raw material condenser are connected with the raw material buffer tank; the raw material delivery pump at the bottom of the raw material buffer tank is connected with a feed inlet of the low-temperature complexing aluminum-removing inlet-outlet heat exchanger; the low-temperature complexing and aluminum removing inlet and outlet heat exchanger feed outlet is connected with the low-temperature cooler inlet; the outlet of the low-temperature cooler is connected with the top of the low-temperature complexing stirring tank; the low-temperature complexing transfer pump at the bottom of the low-temperature complexing stirring tank is connected with a low-temperature complexing stirring tank filter; the bottom of the low-temperature complexing stirring tank filter is connected with a dryer, and the lateral line of the low-temperature complexing and aluminum-removing filter is connected with a discharge inlet of the low-temperature complexing heat exchanger; the outlet of the low-temperature complexing aluminum removal inlet-outlet heat exchanger is connected with the inlet of the liquid-phase aluminum removal preheater; the outlet of the liquid-phase aluminum removal preheater is connected with the top of the liquid-phase aluminum removal tank; the bottom of the liquid phase aluminum removal tank is connected with an evaporation kettle; the top of the evaporation kettle is connected with a gas phase heater; the outlet of the gas phase heater is tightly connected with the bottom of the gas phase aluminum removal column; the top of the gas phase aluminum removal column is connected with a gas phase condenser; the top of the product buffer tank is connected with the outlet of the gas phase condenser, and the bottom of the product buffer tank is connected with a product discharge pump; the inlet of the high-pressure rectifying tower preheater is connected with a product discharge pump, and the outlet of the high-pressure rectifying tower preheater is connected with a high-pressure rectifying tower; the high-pressure rectifying tower comprises a high-pressure rectifying tower condenser and a high-pressure rectifying tower evaporator, and the upper section and the lower section in the tower are random packing or regular packing.
The corresponding simultaneous series connection gas phase complexing aluminum removal process and the process after high-pressure rectification aluminum removal are as follows: feeding a chlorosilane mixture containing aluminum impurities at the top of a stirring and settling tank, settling and separating, drying and separating the tank bottom mixture by a dryer to obtain silicon powder and aluminum slag, and condensing the silicon powder and the aluminum slag by a raw material condenser to enter a raw material buffer tank; the chlorosilane mixture extracted from the side line enters a raw material buffer tank after being filtered and separated by a stirring settling tank filter; the raw materials are pre-cooled in a heat exchanger through low-temperature complexing aluminum removal, and then cooled through a low-temperature cooler to enter a low-temperature complexing stirring tank filled with a low-temperature complexing aluminum removal agent for aluminum removal; filtering and removing aluminum chloride waste residues through a low-temperature complexing stirring tank filter, wherein a chlorosilane mixture filtered by the low-temperature complexing stirring tank filter and a raw material conveyed by a raw material buffer tank are subjected to low-temperature complexing aluminum removal to exchange heat in a heat exchanger, and precooling the raw material; heating chlorosilane through a liquid-phase dealuminization preheater, and feeding the heated chlorosilane into a liquid-phase dealuminization tank filled with a liquid-phase dealuminization agent for dealuminization; evaporating and gasifying liquid chlorosilane subjected to liquid phase dealuminization through an evaporation kettle, heating the liquid chlorosilane through a gas phase heater, introducing the liquid chlorosilane into a gas phase dealuminization column filled with a gas phase complexing dealuminization agent for dealuminization, and condensing the gas phase chlorosilane discharged from the top of the gas phase dealuminization column to be in a liquid state through a gas phase condenser to a product buffer tank; and (3) conveying the condensed chlorosilane to a high-pressure rectifying tower preheater through a product discharge pump, heating, introducing into a high-pressure rectifying tower for high-pressure rectification and aluminum removal, finally separating an aluminum-containing high-boiling-point substance from the bottom of an evaporator of the high-pressure rectifying tower, and condensing and liquefying the purified chlorosilane through a condenser of the high-pressure rectifying tower to obtain a high-purity chlorosilane liquid product after aluminum removal.
When the complexing aluminum-removing equipment runs, a low-temperature complexing aluminum-removing agent is filled in the low-temperature complexing stirring tank; filling a liquid phase aluminum removing agent in the liquid phase aluminum removing tank; filling a gas phase aluminum removing agent in the gas phase aluminum removing column; and the aluminum removing agents are required to be replaced periodically.
The low-temperature complexing aluminum remover and the liquid-phase complexing aluminum remover adopt alkali metal, alkaline earth metal salt or a compound thereof, Lewis base containing nitrogen, oxygen, sulfur and phosphorus or a compound thereof, or a mixture of the above substances, preferably lithium chloride, sodium chloride, potassium chloride and amine compounds.
The gas phase aluminum remover adopts alkali metal, alkaline earth metal salt or a compound thereof loaded by a porous material, and Lewis base containing nitrogen, oxygen, sulfur and phosphorus or a compound thereof loaded by the porous material, preferably lithium chloride, sodium chloride, potassium chloride and amine compounds loaded by the porous material.
The filling amount of the low-temperature complexing aluminum remover and the liquid-phase aluminum remover is 40-50% of the volume of the tank, and the filling height of the gas-phase aluminum remover is 70-80% of the height of the adsorption column. Wherein, the gas phase aluminum remover carrier is active carbon or active alumina material with porous structure, and the loading amount is 5-15% of the carrier mass.
The low-temperature complexing aluminum-removing inlet-outlet heat exchanger precools the raw materials to-10-0 ℃; the low-temperature cooler 8 cools the chlorosilane to a temperature ranging from-20 ℃ to-30 ℃.
The liquid-phase aluminum removal preheater preheats the chlorosilane mixture subjected to low-temperature complexing aluminum removal to 20-30 ℃; the gas phase heater heats chlorosilane mixed steam from the evaporation kettle to 120-140 ℃.
The high-pressure rectifying tower preheater preheats chlorosilane to 180-220 ℃; and the operating pressure of the high-pressure rectifying tower is controlled to be 15-35 atm.
In order to improve the purity of the chlorosilane, the content of aluminum impurities in the chlorosilane is greatly reduced. The invention provides a chlorosilane complexing aluminum removal process and equipment. The aluminum is removed by low-temperature complexing, the content of aluminum chloride in the chlorosilane is further reduced by combining a liquid phase complexing process, and finally the high-purity chlorosilane containing almost no aluminum is obtained by serially connecting a gas phase complexing aluminum removal process and a high-pressure rectification aluminum removal process.
The invention has the following advantages:
(1) the low-temperature complexing aluminum removal process, the liquid-phase complexing aluminum removal process, the gas-phase complexing process and the high-pressure rectification aluminum removal process can be operated independently or in combination to meet different chlorosilane purification requirements.
(2) The chlorosilane mixture filtered by the low-temperature complexing stirring tank filter and the raw material conveyed by the raw material buffer tank are subjected to heat exchange in the low-temperature complexing aluminum-removing heat exchanger, so that the effective utilization of energy is realized.
(3) The low-temperature complexing aluminum remover, the liquid-phase aluminum remover and the gas-phase aluminum remover have longer service life and obvious complexing aluminum removing effect.
(4) The optional complexing aluminum remover has more varieties, and can keep higher complexing aluminum removal performance under the condition of the process operation range.
(5) In order to improve the aluminum removal rate of the chlorosilane, the aluminum chloride content in the chlorosilane is reduced by low-temperature complexing aluminum removal and liquid-phase complexing aluminum removal processes, and finally the aluminum content in the chlorosilane can be reduced to be below 0.001ppm by serially connecting gas-phase complexing aluminum removal and high-pressure rectification aluminum removal processes.
Drawings
FIG. 1 is a schematic flow diagram of a process equipment combining low-temperature complexing and liquid-phase complexing aluminum removal processes. FIG. 2 is a schematic flow diagram of a series-connected process equipment for removing aluminum by gas phase complexation. FIG. 3 is a schematic flow diagram of a series of process equipment for removing aluminum by high-pressure rectification. FIG. 4 is a schematic flow diagram of a series of process equipment for vapor phase complexation aluminum removal and high-pressure rectification aluminum removal.
1-stirring settling tank 2-dryer 3-stirring settling tank filter 4-raw material condenser 5-raw material buffer tank 6-raw material delivery pump 7-low temperature complexing and aluminum removing inlet-outlet heat exchanger 8-low temperature cooler 9-low temperature complexing and stirring tank 10-low temperature complexing and delivery pump 11-low temperature complexing and stirring tank filter 12-liquid phase aluminum removing preheater 13-liquid phase aluminum removing tank 14-product buffer tank 15-product outlet pump 16-gas phase condenser 17-evaporation kettle 18-gas phase heater 19-gas phase aluminum removing column 20-high pressure rectifying tower preheater 21-high pressure rectifying tower 22-high pressure rectifying tower condenser 23-high pressure rectifying tower evaporator
Detailed Description
A detailed description of the preferred embodiments is provided herein. However, it should be understood that the present invention may be embodied in various forms. Therefore, specific details disclosed herein are not to be interpreted as limiting, but rather as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the present invention in virtually any appropriately detailed system, structure, or manner.
The drawings constitute a part of this specification and include exemplary embodiments to the invention, which may be embodied in various forms. It should be understood that aspects of the invention may be exaggerated or enlarged in some instances to facilitate an understanding of the invention.
The process and apparatus provided by the present invention will be further described with reference to FIG. 1.
An apparatus for removing aluminum by chlorosilane complexation comprises: the device comprises a stirring settling tank 1, a dryer 2, a stirring settling tank filter 3, a raw material condenser 4, a raw material buffer tank 5, a raw material delivery pump 6, a low-temperature complexing aluminum-removing inlet-outlet heat exchanger 7, a low-temperature cooler 8, a low-temperature complexing stirring tank 9, a low-temperature complexing delivery pump 10, a low-temperature complexing stirring tank filter 11, a liquid-phase aluminum-removing preheater 12, a liquid-phase aluminum-removing tank 13, a product buffer tank 14 and a product discharge pump 15; wherein the bottom of the stirring and settling tank 1 is connected with a dryer 2, and the lateral line is connected with a stirring and settling tank filter 3; the upper part of the dryer 2 is connected with a raw material condenser 4; the stirring and settling tank filter 3 and the raw material condenser 4 are connected with a raw material buffer tank 5; a raw material delivery pump 6 at the bottom of the raw material buffer tank 5 is connected with a feeding inlet of a low-temperature complexing and aluminum-removing inlet-outlet heat exchanger 7; the feeding outlet of the low-temperature complexing and aluminum removing heat exchanger 7 is connected with the inlet of the low-temperature cooler 8; the outlet of the low-temperature cooler 8 is connected with the top of the low-temperature complexing stirring tank 9; a low-temperature complexing transfer pump 10 at the bottom of the low-temperature complexing stirring tank 9 is connected with a low-temperature complexing stirring tank filter 11; the bottom of the low-temperature complexing stirring tank filter 11 is connected with a dryer 2, and the lateral line of the low-temperature complexing and aluminum-removing filter is connected with a discharge inlet of the low-temperature complexing heat exchanger 7; the outlet of the low-temperature complexing and aluminum removing heat exchanger 7 is connected with the inlet of a liquid-phase aluminum removing preheater 12; the outlet of the liquid phase dealuminization preheater 12 is connected with a liquid phase dealuminization tank 13; the top of the product buffer tank 14 is connected with a liquid phase aluminum removal tank 13, and the bottom is connected with a product discharge pump 15; and pumping out the chlorosilane product after the aluminum is removed by a product discharge pump.
Feeding the liquid chlorosilane mixture discharged by cold hydrogenation at the top of a stirring and settling tank 1, settling and separating, drying and separating the mixture at the bottom of the tank by a dryer 2 to obtain silicon powder and aluminum slag, and condensing the silicon powder and the aluminum slag by a raw material condenser 4 to enter a raw material buffer tank 5; the chlorosilane mixture extracted from the side line is filtered and separated by a stirring settling tank filter 3 and then enters a raw material buffer tank 5; the raw materials are pre-cooled to-10-0 ℃ through a low-temperature complexing and aluminum-removing inlet-outlet heat exchanger 7, cooled to the temperature range of-20 ℃ to-30 ℃ through a low-temperature cooler 8, then enter a low-temperature complexing stirring tank 9 for removing aluminum, and then are filtered through a low-temperature complexing stirring tank filter 11 to remove aluminum chloride waste residues, wherein a chlorosilane mixture filtered through the low-temperature complexing stirring tank filter 11 and the raw materials conveyed by a raw material buffer tank 5 exchange heat through the low-temperature complexing and aluminum-removing inlet-outlet heat exchanger 7, and the raw materials are pre-cooled; chlorosilane is heated to 20-30 ℃ by a liquid phase dealuminization preheater 12 and enters a liquid phase dealuminization tank 13 for dealuminization; liquid chlorosilane subjected to liquid phase aluminum removal enters a product buffer tank 14; and pumping out the chlorosilane through a product discharge pump 15 to obtain a high-purity chlorosilane liquid product after aluminum removal.
Wherein the low-temperature complexing and aluminum removing agent is filled in the low-temperature complexing and stirring tank 9; the liquid phase aluminum removing tank 13 is filled with a liquid phase complexing aluminum removing agent; and the aluminum removing agents are required to be replaced periodically. The filling amount of the low-temperature complexing aluminum remover and the liquid-phase complexing aluminum remover is 40-50% of the volume of the tank.
In order to improve the aluminum removal rate of the chlorosilane, the aluminum chloride content in the chlorosilane can be reduced to 0.01ppm-0.1ppm by low-temperature complexing aluminum removal and liquid-phase complexing aluminum removal processes.
Example 1:
the low-temperature complexing aluminum remover and the liquid-phase complexing aluminum remover adopt sodium chloride, and the filling amount is 40 percent of the volume of the tank.
Feeding a mixture raw material containing 10ppm of aluminum chloride at the top of a stirring and settling tank at 20 ℃, settling and separating, drying and separating the mixture at the bottom of the tank by a dryer to obtain silicon powder and aluminum slag, condensing by a raw material condenser and feeding into a raw material buffer tank; the chlorosilane mixture extracted from the side line enters a raw material buffer tank after being filtered and separated by a stirring settling tank filter; the raw materials are subjected to low-temperature complexing dealumination, enter a heat exchanger and are pre-cooled to-5 ℃, then are cooled to-30 ℃ by a low-temperature cooler, enter a low-temperature complexing stirring tank filled with sodium chloride to remove aluminum, and then are filtered by a low-temperature complexing stirring tank filter to remove aluminum chloride waste residues; heating the chlorosilane subjected to low-temperature complexing and aluminum removal to 20 ℃ through a liquid-phase aluminum removal preheater, and allowing the chlorosilane to enter a liquid-phase aluminum removal tank filled with sodium chloride for aluminum removal; liquid chlorosilane subjected to liquid phase aluminum removal enters a product buffer tank; the aluminum content of the chlorosilane product in the detection tank is 0.026 ppm.
Example 2:
the low-temperature complexing aluminum remover and the liquid-phase complexing aluminum remover adopt dimethylamine hydrochloride, and the filling amount is 50 percent of the volume of the tank.
Feeding a mixture raw material containing 10ppm of aluminum chloride at the top of a stirring and settling tank at 20 ℃, settling and separating, drying and separating the mixture at the bottom of the tank by a dryer to obtain silicon powder and aluminum slag, condensing by a raw material condenser and feeding into a raw material buffer tank; the chlorosilane mixture extracted from the side line enters a raw material buffer tank after being filtered and separated by a stirring settling tank filter; the raw materials are pre-cooled to 0 ℃ through a low-temperature complexing and aluminum-removing heat exchanger, cooled to-20 ℃ through a low-temperature cooler, enter a low-temperature complexing stirring tank filled with dimethylamine hydrochloride to remove aluminum, and then are filtered through a low-temperature complexing stirring tank filter to remove aluminum chloride waste residues; heating the chlorosilane subjected to low-temperature complexing and aluminum removal to 30 ℃ through a liquid-phase aluminum removal preheater, and allowing the chlorosilane to enter a liquid-phase aluminum removal tank filled with dimethylamine hydrochloride for aluminum removal; liquid chlorosilane subjected to liquid phase aluminum removal enters a product buffer tank; the content of the aluminum chlorosilicate in the detection tank is 0.018 ppm.
The process and apparatus provided by the present invention will be further described with reference to FIG. 2.
The chlorosilane aluminum removal equipment of the series gas-phase complexing aluminum removal process comprises: the device comprises a stirring settling tank 1, a dryer 2, a stirring settling tank filter 3, a raw material condenser 4, a raw material buffer tank 5, a raw material delivery pump 6, a low-temperature complexing aluminum-removing inlet-outlet heat exchanger 7, a low-temperature cooler 8, a low-temperature complexing stirring tank 9, a low-temperature complexing delivery pump 10, a low-temperature complexing stirring tank filter 11, a liquid-phase aluminum-removing preheater 12, a liquid-phase aluminum-removing tank 13, a product buffer tank 14, a product discharge pump 15, a gas-phase condenser 16, an evaporation kettle 17, a gas-phase heater 18 and a gas-phase aluminum-removing column 19; wherein the bottom of the stirring and settling tank 1 is connected with a dryer 2, and the lateral line is connected with a stirring and settling tank filter 3; the upper part of the dryer 2 is connected with a raw material condenser 4; the stirring and settling tank filter 3 and the raw material condenser 4 are connected with a raw material buffer tank 5; a raw material delivery pump 6 at the bottom of the raw material buffer tank 5 is connected with a feeding inlet of a low-temperature complexing and aluminum-removing inlet-outlet heat exchanger 7; the feeding outlet of the low-temperature complexing and aluminum removing heat exchanger 7 is connected with the inlet of the low-temperature cooler 8; the outlet of the low-temperature cooler 8 is connected with the top of the low-temperature complexing stirring tank 9; a low-temperature complexing transfer pump 10 at the bottom of the low-temperature complexing stirring tank 9 is connected with a low-temperature complexing stirring tank filter 11; the bottom of the low-temperature complexing stirring tank filter 11 is connected with a dryer 2, and the lateral line of the low-temperature complexing and aluminum-removing filter is connected with a discharge inlet of the low-temperature complexing heat exchanger 7; the outlet of the low-temperature complexing and aluminum removing heat exchanger 7 is connected with the inlet of a liquid-phase aluminum removing preheater 12; the outlet of the liquid phase aluminum removal preheater 12 is connected with the top of the liquid phase aluminum removal tank 13; at the moment, the bottom of the liquid phase aluminum removal tank 13 is connected with an evaporation kettle 17; the evaporation kettle 17 is connected with an inlet of a gas phase heater 18; the outlet of the gas-phase heater 18 is connected with the bottom of a gas-phase aluminum removal column 19; the top of the gas phase aluminum removal column 19 is connected with an inlet of a gas phase condenser 16; the outlet of the gas phase condenser 16 is connected with the top of the product buffer tank 14; the bottom of the product buffer tank 14 is connected with a product discharge pump 15; and pumping out the chlorosilane product after the aluminum is removed by a product discharge pump.
Feeding the liquid chlorosilane mixture discharged by cold hydrogenation at the top of a stirring and settling tank 1, settling and separating, drying and separating the mixture at the bottom of the tank by a dryer 2 to obtain silicon powder and aluminum slag, and condensing the silicon powder and the aluminum slag by a raw material condenser 4 to enter a raw material buffer tank 5; the chlorosilane mixture extracted from the side line is filtered and separated by a stirring settling tank filter 3 and then enters a raw material buffer tank 5; the raw materials are pre-cooled to-10-0 ℃ through a low-temperature complexing and aluminum-removing inlet-outlet heat exchanger 7, cooled to the temperature range of-20 ℃ to-30 ℃ through a low-temperature cooler 8, then enter a low-temperature complexing stirring tank 9 for removing aluminum, and then are filtered through a low-temperature complexing stirring tank filter 11 to remove aluminum chloride waste residues, wherein a chlorosilane mixture filtered through the low-temperature complexing stirring tank filter 11 and the raw materials conveyed by a raw material buffer tank 5 exchange heat through the low-temperature complexing and aluminum-removing inlet-outlet heat exchanger 7, and the raw materials are pre-cooled; chlorosilane is heated to 20-30 ℃ by a liquid phase dealuminization preheater 12 and enters a liquid phase dealuminization tank 13 for dealuminization; evaporating and gasifying liquid chlorosilane subjected to liquid phase dealuminization in an evaporation kettle 17, heating the liquid chlorosilane to 120-140 ℃ by using a gas phase heater 18, introducing the liquid chlorosilane into a gas phase dealuminization column 19 for dealuminization; chlorosilane discharged from the top is condensed to be liquid through a gas phase condenser 16 and then is sent to a product buffer tank 14; and pumping out the chlorosilane through a product discharge pump 15 to obtain a high-purity chlorosilane liquid product after aluminum removal.
Wherein the low-temperature complexing and aluminum removing agent is filled in the low-temperature complexing and stirring tank 9; the liquid phase aluminum removing tank 13 is filled with a liquid phase aluminum removing agent; the gas phase aluminum removing column 19 is filled with a gas phase complexing aluminum removing agent; and the aluminum removing agents are required to be replaced periodically. The filling amount of the low-temperature complexing aluminum remover and the liquid-phase complexing aluminum remover is 40-50% of the volume of the tank; the filling height of the gas phase aluminum removing agent is 70-80% of the height of the adsorption column.
In order to improve the aluminum removal rate of the chlorosilane, the aluminum chloride content in the chlorosilane can be reduced to 0.001ppm-0.01ppm by connecting a low-temperature complexing aluminum removal process and a liquid-phase complexing aluminum removal process in series with a gas-phase complexing aluminum removal process.
Example 3:
the low-temperature complexing aluminum remover and the liquid-phase complexing aluminum remover are potassium chloride, and the gas-phase complexing aluminum remover is a mixture (mixed by equal mass, and the total mass fraction of the load is 10%) of dimethylamine hydrochloride and sodium chloride loaded by active alumina.
Feeding a mixture raw material containing 10ppm of aluminum chloride at the top of a stirring and settling tank at 20 ℃, settling and separating, drying and separating the mixture at the bottom of the tank by a dryer to obtain silicon powder and aluminum slag, condensing by a raw material condenser and feeding into a raw material buffer tank; the chlorosilane mixture extracted from the side line enters a raw material buffer tank after being filtered and separated by a stirring settling tank filter; the raw materials are pre-cooled to-5 ℃ through a low-temperature complexing dealuminization heat exchanger, cooled to-30 ℃ through a low-temperature cooler, enter a low-temperature complexing stirring tank filled with a potassium chloride dealuminization agent for dealuminization, heated to 20 ℃ through a liquid-phase dealuminization preheater, enter a liquid-phase dealuminization tank for dealuminization, and added with the potassium chloride dealuminization agent; evaporating and gasifying liquid chlorosilane in an evaporation kettle, heating the liquid chlorosilane to 140 ℃ through a gas phase heater, introducing a gas phase aluminum removal column filled with dimethylamine hydrochloride and sodium chloride loaded by activated alumina for removing aluminum; condensing chlorosilane discharged from the top to be in a liquid state through a gas phase condenser and sending the liquid to a product buffer tank; the aluminum content of the chlorosilane product in the detection tank is 0.0034 ppm.
Example 4:
the low-temperature complexing aluminum remover and the liquid-phase complexing aluminum remover are selected from a mixture (equal molar mixing) of lithium chloride and potassium chloride, and the gas-phase complexing aluminum remover is selected from dimethylamine hydrochloride loaded by activated carbon (equal mass mixing, the loading mass fraction is 15%).
Feeding a mixture raw material containing 10ppm of aluminum chloride at the top of a stirring and settling tank at 20 ℃, settling and separating, drying and separating the mixture at the bottom of the tank by a dryer to obtain silicon powder and aluminum slag, condensing by a raw material condenser and feeding into a raw material buffer tank; the chlorosilane mixture extracted from the side line enters a raw material buffer tank after being filtered and separated by a stirring settling tank filter; the raw materials are pre-cooled to 0 ℃ through a low-temperature complexing dealuminization heat exchanger, cooled to-20 ℃ through a low-temperature cooler, enter a low-temperature complexing stirring tank filled with lithium chloride and potassium chloride dealuminization agents to remove aluminum, heated to 30 ℃ through a liquid-phase dealuminization preheater, enter a liquid-phase dealuminization tank to remove aluminum, and added with the lithium chloride and potassium chloride dealuminization agents; evaporating and gasifying liquid chlorosilane in an evaporation kettle, heating the liquid chlorosilane to 130 ℃ through a gas phase heater, and introducing a gas phase aluminum removal column filled with activated carbon-loaded dimethylamine hydrochloride to remove aluminum; condensing chlorosilane discharged from the top to be in a liquid state through a gas phase condenser and sending the liquid to a product buffer tank; the aluminum content of the chlorosilane product in the detection tank is 0.0022 ppm.
The process and apparatus provided by the present invention will be further described with reference to FIG. 3.
The chlorosilane aluminum removal equipment of the series high-pressure rectification aluminum removal process comprises: the device comprises a stirring settling tank 1, a dryer 2, a stirring settling tank filter 3, a raw material condenser 4, a raw material buffer tank 5, a raw material delivery pump 6, a low-temperature complexing and dealuminizing inlet-outlet heat exchanger 7, a low-temperature cooler 8, a low-temperature complexing and stirring tank 9, a low-temperature complexing and delivery pump 10, a low-temperature complexing and stirring tank filter 11, a liquid-phase dealuminizing preheater 12, a liquid-phase dealuminizing tank 13, a product buffer tank 14, a product discharge pump 15, a high-pressure rectifying tower preheater 20, a high-pressure rectifying tower 21, a high-pressure rectifying tower condenser 22 and a high-pressure rectifying tower evaporator 23; wherein the bottom of the stirring and settling tank 1 is connected with a dryer 2, and the lateral line is connected with a stirring and settling tank filter 3; the upper part of the dryer 2 is connected with a raw material condenser 4; the stirring and settling tank filter 3 and the raw material condenser 4 are connected with a raw material buffer tank 5; a raw material delivery pump 6 at the bottom of the raw material buffer tank 5 is connected with a feeding inlet of a low-temperature complexing and aluminum-removing inlet-outlet heat exchanger 7; the feeding outlet of the low-temperature complexing and aluminum removing heat exchanger 7 is connected with the inlet of the low-temperature cooler 8; the outlet of the low-temperature cooler 8 is connected with the top of the low-temperature complexing stirring tank 9; a low-temperature complexing transfer pump 10 at the bottom of the low-temperature complexing stirring tank 9 is connected with a low-temperature complexing stirring tank filter 11; the bottom of the low-temperature complexing stirring tank filter 11 is connected with a dryer 2, and the lateral line of the low-temperature complexing and aluminum-removing filter is connected with a discharge inlet of the low-temperature complexing heat exchanger 7; the outlet of the low-temperature complexing and aluminum removing heat exchanger 7 is connected with the inlet of a liquid-phase aluminum removing preheater 12; the outlet of the liquid phase aluminum removal preheater 12 is connected with the top of the liquid phase aluminum removal tank 13; the bottom of the liquid phase aluminum removal tank 13 is connected with the top of a product buffer tank 14; the bottom of the product buffer tank 14 is connected with a product discharge pump 15; at the moment, the product discharge pump 15 is connected with the inlet of the high-pressure rectifying tower preheater 20; the outlet of the high-pressure rectifying tower preheater 20 is connected with the middle feeding position of the high-pressure rectifying tower 21; the high pressure rectification column has an overhead condenser 22 and a bottom evaporator 23. The overhead condenser 22 condenses and extracts the chlorosilane liquid product after the aluminum is removed.
Feeding the liquid chlorosilane mixture discharged by cold hydrogenation at the top of a stirring and settling tank 1, settling and separating, drying and separating the mixture at the bottom of the tank by a dryer 2 to obtain silicon powder and aluminum slag, and condensing the silicon powder and the aluminum slag by a raw material condenser 4 to enter a raw material buffer tank 5; the chlorosilane mixture extracted from the side line is filtered and separated by a stirring settling tank filter 3 and then enters a raw material buffer tank 5; the raw materials are pre-cooled to-10-0 ℃ through a low-temperature complexing and aluminum-removing inlet-outlet heat exchanger 7, cooled to the temperature range of-20 ℃ to-30 ℃ through a low-temperature cooler 8, then enter a low-temperature complexing stirring tank 9 for removing aluminum, and then are filtered through a low-temperature complexing stirring tank filter 11 to remove aluminum chloride waste residues, wherein a chlorosilane mixture filtered through the low-temperature complexing stirring tank filter 11 and the raw materials conveyed by a raw material buffer tank 5 exchange heat through the low-temperature complexing and aluminum-removing inlet-outlet heat exchanger 7, and the raw materials are pre-cooled; chlorosilane is heated to 20-30 ℃ by a liquid phase dealuminization preheater 12 and enters a liquid phase dealuminization tank 13 for dealuminization; liquid chlorosilane subjected to liquid phase aluminum removal enters a product buffer tank 14; conveying the chlorosilane in the tank to a high-pressure rectifying tower preheater 20 through a product discharge pump 15, heating to 180-220 ℃, introducing the chlorosilane into a high-pressure rectifying tower 21 for high-pressure rectification to remove aluminum, controlling the pressure to be 15-35atm, finally separating aluminum-containing high-boiling-point substances from the bottom of a high-pressure rectifying tower evaporator 23, and condensing and liquefying the purified chlorosilane through a high-pressure rectifying tower condenser 22 to obtain a high-purity chlorosilane liquid product after aluminum removal.
Wherein the low-temperature complexing and aluminum removing agent is filled in the low-temperature complexing and stirring tank 9; the liquid phase aluminum removing tank 13 is filled with a liquid phase complexing aluminum removing agent; and the aluminum removing agents are required to be replaced periodically. The filling amount of the low-temperature complexing aluminum remover and the liquid-phase complexing aluminum remover is 40-50% of the volume of the tank.
In order to improve the aluminum removal rate of the chlorosilane, the aluminum chloride content in the chlorosilane can be reduced to 0.001ppm-0.01ppm by connecting a low-temperature complexing aluminum removal process and a liquid-phase complexing aluminum removal process in series with a high-pressure rectification aluminum removal process.
Example 5:
the low-temperature complexing aluminum remover and the liquid-phase complexing aluminum remover are potassium chloride; the operating pressure of the high-pressure rectifying tower is 20 atm.
Feeding a mixture raw material containing 10ppm of aluminum chloride at the top of a stirring and settling tank at 20 ℃, settling and separating, drying and separating the mixture at the bottom of the tank by a dryer to obtain silicon powder and aluminum slag, condensing by a raw material condenser and feeding into a raw material buffer tank; the chlorosilane mixture extracted from the side line enters a raw material buffer tank after being filtered and separated by a stirring settling tank filter; the raw materials are pre-cooled to-5 ℃ through a low-temperature complexing and aluminum removing heat exchanger, cooled to-30 ℃ through a low-temperature cooler, enter a low-temperature complexing stirring tank filled with potassium chloride for aluminum removal, heated to 20 ℃ through a liquid-phase aluminum removing preheater, enter a liquid-phase aluminum removing tank for aluminum removal, and potassium chloride is added into the tank; conveying the chlorosilane subjected to liquid-phase aluminum removal to a product buffer tank; pumping chlorosilane into a high-pressure rectifying tower preheater by using a product discharging pump, heating to 180 ℃, introducing into a high-pressure rectifying tower with the operating pressure of 20atm for high-pressure rectifying and aluminum removing operation, finally condensing and liquefying by using a condenser of the high-pressure rectifying tower to obtain a high-purity chlorosilane liquid product after aluminum removal, and detecting the aluminum content of the chlorosilane product to be 0.0043 ppm.
Example 6:
the low-temperature complexing aluminum remover and the liquid-phase complexing aluminum remover are prepared by mixing potassium chloride and dimethylamine hydrochloride in equal molar ratio; the operating pressure of the high-pressure rectifying tower is 30 atm.
Feeding a mixture raw material containing 10ppm of aluminum chloride at the top of a stirring and settling tank at 20 ℃, settling and separating, drying and separating the mixture at the bottom of the tank by a dryer to obtain silicon powder and aluminum slag, condensing by a raw material condenser and feeding into a raw material buffer tank; the chlorosilane mixture extracted from the side line enters a raw material buffer tank after being filtered and separated by a stirring settling tank filter; the raw materials are pre-cooled to 0 ℃ through a low-temperature complexing and dealuminizing inlet-outlet heat exchanger, cooled to-25 ℃ through a low-temperature cooler, enter a low-temperature complexing stirring tank filled with potassium chloride and dimethylamine hydrochloride for dealuminizing, heated to 25 ℃ through a liquid-phase dealuminizing preheater, enter a liquid-phase dealuminizing tank for dealuminizing, and added with the potassium chloride and the dimethylamine hydrochloride; conveying the chlorosilane subjected to liquid-phase aluminum removal to a product buffer tank; pumping chlorosilane into a high-pressure rectifying tower preheater by using a product discharge pump, heating to 200 ℃, introducing into a high-pressure rectifying tower with the operating pressure of 30atm for high-pressure rectifying and aluminum removing operation, and finally condensing and liquefying by using a condenser of the high-pressure rectifying tower to obtain a high-purity chlorosilane liquid product after aluminum removal, wherein the detected aluminum content of the chlorosilane product is 0.0038 ppm.
The process and apparatus provided by the present invention will be further described with reference to FIG. 4.
The chlorosilane aluminum removal equipment for the simultaneous series connection of the gas phase complexing aluminum removal process and the high-pressure rectification aluminum removal process comprises: the device comprises a stirring settling tank 1, a dryer 2, a stirring settling tank filter 3, a raw material condenser 4, a raw material buffer tank 5, a raw material delivery pump 6, a low-temperature complexing aluminum removal inlet-outlet heat exchanger 7, a low-temperature cooler 8, a low-temperature complexing stirring tank 9, a low-temperature complexing delivery pump 10, a low-temperature complexing stirring tank filter 11, a liquid-phase aluminum removal preheater 12, a liquid-phase aluminum removal tank 13, a product buffer tank 14, a product discharge pump 15, a gas-phase condenser 16, an evaporation kettle 17, a gas-phase heater 18, a gas-phase aluminum removal column 19, a high-pressure rectifying tower preheater 20, a high-pressure rectifying tower 21, a high-pressure rectifying tower condenser 22 and a high-pressure rectifying tower; wherein the bottom of the stirring and settling tank 1 is connected with a dryer 2, and the lateral line is connected with a stirring and settling tank filter 3; the upper part of the dryer 2 is connected with a raw material condenser 4; the stirring and settling tank filter 3 and the raw material condenser 4 are connected with a raw material buffer tank 5; a raw material delivery pump 6 at the bottom of the raw material buffer tank 5 is connected with a feeding inlet of a low-temperature complexing and aluminum-removing inlet-outlet heat exchanger 7; the feeding outlet of the low-temperature complexing and aluminum removing heat exchanger 7 is connected with the inlet of the low-temperature cooler 8; the outlet of the low-temperature cooler 8 is connected with the top of the low-temperature complexing stirring tank 9; a low-temperature complexing transfer pump 10 at the bottom of the low-temperature complexing stirring tank 9 is connected with a low-temperature complexing stirring tank filter 11; the bottom of the low-temperature complexing stirring tank filter 11 is connected with a dryer 2, and the lateral line of the low-temperature complexing and aluminum-removing filter is connected with a discharge inlet of the low-temperature complexing heat exchanger 7; the outlet of the low-temperature complexing and aluminum removing heat exchanger 7 is connected with the inlet of a liquid-phase aluminum removing preheater 12; the outlet of the liquid phase aluminum removal preheater 12 is connected with the top of the liquid phase aluminum removal tank 13; the bottom of the liquid phase aluminum removal tank 13 is connected with an evaporation kettle 17; the evaporation kettle 17 is connected with an inlet of a gas phase heater 18; the outlet of the gas-phase heater 18 is connected with the bottom of a gas-phase aluminum removal column 19; the top of the gas phase aluminum removal column 19 is connected with an inlet of a gas phase condenser 16; the outlet of the gas phase condenser 16 is connected with the top of the product buffer tank 14; the bottom of the product buffer tank 14 is connected with a product discharge pump 15; at the moment, the product discharge pump 15 is connected with the inlet of the high-pressure rectifying tower preheater 20; the outlet of the high-pressure rectifying tower preheater 20 is connected with the middle feeding position of the high-pressure rectifying tower 21; the high pressure rectification column has an overhead condenser 22 and a bottom evaporator 23. The overhead condenser 22 condenses and extracts the chlorosilane liquid product after the aluminum is removed.
Feeding the liquid chlorosilane mixture discharged by cold hydrogenation at the top of a stirring and settling tank 1, settling and separating, drying and separating the mixture at the bottom of the tank by a dryer 2 to obtain silicon powder and aluminum slag, and condensing the silicon powder and the aluminum slag by a raw material condenser 4 to enter a raw material buffer tank 5; the chlorosilane mixture extracted from the side line is filtered and separated by a stirring settling tank filter 3 and then enters a raw material buffer tank 5; the raw materials are pre-cooled to-10-0 ℃ through a low-temperature complexing and aluminum-removing inlet-outlet heat exchanger 7, cooled to the temperature range of-20 ℃ to-30 ℃ through a low-temperature cooler 8, then enter a low-temperature complexing stirring tank 9 for removing aluminum, and then are filtered through a low-temperature complexing stirring tank filter 11 to remove aluminum chloride waste residues, wherein a chlorosilane mixture filtered through the low-temperature complexing stirring tank filter 11 and the raw materials conveyed by a raw material buffer tank 5 exchange heat through the low-temperature complexing and aluminum-removing inlet-outlet heat exchanger 7, and the raw materials are pre-cooled; chlorosilane is heated to 20-30 ℃ by a liquid phase dealuminization preheater 12 and enters a liquid phase dealuminization tank 13 for dealuminization; evaporating and gasifying liquid chlorosilane subjected to liquid phase dealuminization in an evaporation kettle 17, heating the liquid chlorosilane to 120-140 ℃ by using a gas phase heater 18, introducing the liquid chlorosilane into a gas phase dealuminization column 19 for dealuminization; chlorosilane discharged from the top is condensed to be liquid through a gas phase condenser 16 and then is sent to a product buffer tank 14; and (3) conveying the chlorosilane in the tank to a high-pressure rectifying tower preheater 20 by a product discharge pump 15, heating to 180-220 ℃, introducing into a high-pressure rectifying tower 21 for high-pressure rectification and aluminum removal, controlling the pressure to be 15-35atm, finally separating aluminum-containing high-boiling-point substances from the bottom of a high-pressure rectifying tower evaporator 23, and condensing and liquefying the purified chlorosilane by a high-pressure rectifying tower condenser 22 to obtain a high-purity chlorosilane liquid product after aluminum removal.
Wherein the low-temperature complexing and aluminum removing agent is filled in the low-temperature complexing and stirring tank 9; the liquid phase aluminum removing tank 13 is filled with a liquid phase complexing aluminum removing agent; the gas phase aluminum removing column 19 is filled with a gas phase complexing aluminum removing agent; and the aluminum removing agents are required to be replaced periodically. The filling amount of the low-temperature complexing aluminum remover and the liquid-phase aluminum remover is 40-50% of the volume of the tank; the filling height of the gas phase aluminum removing agent is 70-80% of the height of the adsorption column.
In order to improve the aluminum removal rate of the chlorosilane, the aluminum chloride content in the chlorosilane can be reduced to be below 0.001ppm by simultaneously connecting a low-temperature complexing aluminum removal process and a liquid-phase complexing aluminum removal process in series with a gas-phase complexing aluminum removal process and a high-pressure rectifying aluminum removal process.
Example 7:
lithium chloride is selected as a low-temperature complexing aluminum remover and a liquid-phase complexing aluminum remover, and a mixture (equal mass, total load mass fraction is 15%) of dimethylamine hydrochloride and potassium chloride loaded by active alumina is selected as a gas-phase complexing aluminum remover; the operating pressure of the high-pressure rectifying tower is 20 atm.
Feeding a mixture raw material containing 10ppm of aluminum chloride at the top of a stirring and settling tank at 20 ℃, settling and separating, drying and separating the mixture at the bottom of the tank by a dryer to obtain silicon powder and aluminum slag, condensing by a raw material condenser and feeding into a raw material buffer tank; the chlorosilane mixture extracted from the side line enters a raw material buffer tank after being filtered and separated by a stirring settling tank filter; the raw materials are firstly subjected to low-temperature complexing dealumination, enter a heat exchanger and are pre-cooled to-5 ℃, then are cooled to-30 ℃ by a low-temperature cooler, enter a low-temperature complexing stirring tank filled with lithium chloride for dealumination, are heated to 20 ℃ by a liquid-phase dealumination preheater, enter a liquid-phase dealumination tank for dealumination, and are added with lithium chloride; evaporating and gasifying liquid chlorosilane subjected to liquid phase aluminum removal through an evaporation kettle, heating to 140 ℃ through a gas phase heater, and introducing a gas phase aluminum removal column filled with a mixture of dimethylamine hydrochloride and potassium chloride loaded by activated alumina for aluminum removal; condensing chlorosilane discharged from the top to be in a liquid state through a gas phase condenser and sending the liquid to a product buffer tank; pumping chlorosilane into a high-pressure rectifying tower preheater by using a product discharge pump, heating to 180 ℃, introducing into a high-pressure rectifying tower with the operating pressure of 20atm for high-pressure rectifying and aluminum removing operation, finally condensing and liquefying by using a condenser of the high-pressure rectifying tower to obtain a high-purity chlorosilane liquid product after aluminum removal, and detecting the aluminum content of the chlorosilane product to be 0.00028 ppm.
Example 8:
the low-temperature complexing aluminum remover and the liquid-phase complexing aluminum remover are selected from a mixture of lithium chloride and potassium chloride (equal molar mixing), and the gas-phase complexing aluminum remover is selected from a mixture of dimethylamine hydrochloride and sodium chloride (equal mass mixing, the total mass fraction of the load is 10%) loaded by activated carbon; the operating pressure of the high-pressure rectifying tower is 30 atm.
Feeding a mixture raw material containing 10ppm of aluminum chloride at the top of a stirring and settling tank at 20 ℃, settling and separating, drying and separating the mixture at the bottom of the tank by a dryer to obtain silicon powder and aluminum slag, condensing by a raw material condenser and feeding into a raw material buffer tank; the chlorosilane mixture extracted from the side line enters a raw material buffer tank after being filtered and separated by a stirring settling tank filter; the raw materials are pre-cooled to 0 ℃ through a low-temperature complexing and dealuminizing inlet-outlet heat exchanger, cooled to-20 ℃ through a low-temperature cooler, enter a low-temperature complexing stirring tank filled with lithium chloride and potassium chloride for dealuminizing, heated to 30 ℃ through a liquid-phase dealuminizing preheater, enter a liquid-phase dealuminizing tank for dealuminizing, and added with the lithium chloride and the potassium chloride; evaporating and gasifying liquid chlorosilane subjected to liquid phase dealuminization through an evaporation kettle, heating to 120 ℃ through a gas phase heater, and introducing a gas phase dealuminization column filled with activated carbon-loaded dimethylamine hydrochloride and sodium chloride for dealuminization; condensing chlorosilane discharged from the top to be in a liquid state through a gas phase condenser and sending the liquid to a product buffer tank; pumping chlorosilane into a high-pressure rectifying tower preheater by using a product discharge pump, heating to 200 ℃, introducing into a high-pressure rectifying tower with the operating pressure of 30atm for high-pressure rectifying and aluminum removing operation, finally condensing and liquefying by using a condenser of the high-pressure rectifying tower to obtain a high-purity chlorosilane liquid product after aluminum removal, and detecting the aluminum content of the chlorosilane product to be 0.00012 ppm.
While the present invention has been described with reference to certain embodiments, it will be apparent to one skilled in the art that the present invention may be practiced by modifying, or by suitably modifying and combining, the systems and methods described herein without departing from the spirit, scope, and spirit of the invention. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and content of the invention.
Claims (10)
1. An apparatus for removing aluminum by chlorosilane complexation is characterized by comprising: the system comprises a stirring settling tank, a dryer, a stirring settling tank filter, a raw material condenser, a raw material buffer tank, a raw material delivery pump, a low-temperature complexing and aluminum-removing inlet and outlet heat exchanger, a low-temperature cooler, a low-temperature complexing and stirring tank filter, a low-temperature complexing and delivery pump, a liquid-phase aluminum-removing preheater, a liquid-phase aluminum-removing tank, a product buffer tank and a product discharge pump; wherein the bottom of the stirring and settling tank is connected with a dryer, and the lateral line of the stirring and settling tank is connected with a stirring and settling tank filter; the upper part of the dryer is connected with a raw material condenser; the bottom of the stirring and settling tank filter and the outlet of the raw material condenser are connected with a raw material buffer tank; the raw material delivery pump at the bottom of the raw material buffer tank is connected with a feed inlet of the low-temperature complexing aluminum-removing inlet-outlet heat exchanger; the low-temperature complexing and aluminum removing inlet and outlet heat exchanger feed outlet is connected with the low-temperature cooler inlet; the outlet of the low-temperature cooler is connected with the top of the low-temperature complexing stirring tank; the low-temperature complexing transfer pump at the bottom of the low-temperature complexing stirring tank is connected with a low-temperature complexing stirring tank filter; the bottom of the low-temperature complexing stirring tank filter is connected with a dryer, and the lateral line of the low-temperature complexing and aluminum-removing filter is connected with a discharge inlet of the low-temperature complexing heat exchanger; the outlet of the low-temperature complexing aluminum removal inlet-outlet heat exchanger is connected with the inlet of the liquid-phase aluminum removal preheater; the outlet of the liquid-phase aluminum removal preheater is connected with a liquid-phase aluminum removal tank; the top of the product buffer tank is connected with a liquid phase aluminum removal tank, and the bottom of the product buffer tank is connected with a product discharge pump; and pumping out the chlorosilane product after the aluminum is removed by a product discharge pump.
2. The apparatus for removing aluminum by chlorosilane complex as claimed in claim 1, which comprises an evaporation kettle, a gas phase heater, a gas phase aluminum removal column and a gas phase condenser; realizing the series connection of the low-temperature complexing and liquid-phase complexing aluminum-removing process and the gas-phase complexing aluminum-removing process; wherein the bottom of the stirring and settling tank is connected with a dryer, and the lateral line of the stirring and settling tank is connected with a stirring and settling tank filter; the upper part of the dryer is connected with a raw material condenser; the stirring settling tank filter and the raw material condenser are connected with the raw material buffer tank; the raw material delivery pump at the bottom of the raw material buffer tank is connected with a feed inlet of the low-temperature complexing aluminum-removing inlet-outlet heat exchanger; the low-temperature complexing and aluminum removing inlet and outlet heat exchanger feed outlet is connected with the low-temperature cooler inlet; the outlet of the low-temperature cooler is connected with the top of the low-temperature complexing stirring tank; the low-temperature complexing transfer pump at the bottom of the low-temperature complexing stirring tank is connected with a low-temperature complexing stirring tank filter; the bottom of the low-temperature complexing stirring tank filter is connected with a dryer, and the lateral line of the low-temperature complexing and aluminum-removing filter is connected with a discharge inlet of the low-temperature complexing heat exchanger; the outlet of the low-temperature complexing aluminum removal inlet-outlet heat exchanger is connected with the inlet of the liquid-phase aluminum removal preheater; the outlet of the liquid-phase aluminum removal preheater is connected with a liquid-phase aluminum removal tank; at the moment, the bottom of the liquid phase aluminum removal tank is connected with an evaporation kettle; the evaporation kettle is connected with the inlet of the gas phase heater; the outlet of the gas phase heater is connected with the bottom of the gas phase aluminum removal column; the top of the gas phase aluminum removal column is connected with the inlet of a gas phase condenser; the outlet of the gas phase condenser is connected with a product buffer tank; and the chlorosilane products in the tank are pumped out by a product discharge pump and transported outside.
3. The apparatus for complex removal of aluminum from chlorosilanes as claimed in claim 2, comprising a high-pressure rectification column preheater, a high-pressure rectification column; a high-pressure rectifying tower condenser and a high-pressure rectifying tower evaporator; the low-temperature complexing and liquid-phase complexing aluminum removal process and the high-pressure rectification aluminum removal process are connected in series; wherein the bottom of the stirring and settling tank is connected with a dryer, and the lateral line of the stirring and settling tank is connected with a stirring and settling tank filter; the upper part of the dryer is connected with a raw material condenser; the stirring settling tank filter and the raw material condenser are connected with the raw material buffer tank; the raw material delivery pump at the bottom of the raw material buffer tank is connected with a feed inlet of the low-temperature complexing aluminum-removing inlet-outlet heat exchanger; the low-temperature complexing and aluminum removing inlet and outlet heat exchanger feed outlet is connected with the low-temperature cooler inlet; the outlet of the low-temperature cooler is connected with the top of the low-temperature complexing stirring tank; the low-temperature complexing transfer pump at the bottom of the low-temperature complexing stirring tank is connected with a low-temperature complexing stirring tank filter; the bottom of the low-temperature complexing stirring tank filter is connected with a dryer, and the lateral line of the low-temperature complexing and aluminum-removing filter is connected with a discharge inlet of the low-temperature complexing heat exchanger; the outlet of the low-temperature complexing aluminum removal inlet-outlet heat exchanger is connected with the inlet of the liquid-phase aluminum removal preheater; the outlet of the liquid-phase aluminum removal preheater is connected with a liquid-phase aluminum removal tank; the top of the product buffer tank is connected with a liquid phase aluminum removal tank, and the bottom of the product buffer tank is connected with a product discharge pump; at the moment, the product discharge pump is connected with the inlet of a high-pressure rectifying tower preheater; the outlet of the high-pressure rectifying tower preheater is connected with the middle feeding position of the high-pressure rectifying tower; the high-pressure rectifying tower is provided with a tower top condenser and a tower bottom evaporator.
4. The apparatus for complex dealuminization of chlorosilane as claimed in claim 3, which is characterized by comprising an evaporation kettle, a gas phase heater, a gas phase dealuminization column, a gas phase condenser, a high pressure rectifying tower preheater and a high pressure rectifying tower; a high-pressure rectifying tower condenser and a high-pressure rectifying tower evaporator; the simultaneous series connection of the low-temperature complexing and liquid-phase complexing aluminum-removing process and the gas-phase complexing aluminum-removing and high-pressure rectifying aluminum-removing process is realized; wherein the bottom of the stirring and settling tank is connected with a dryer, and the lateral line of the stirring and settling tank is connected with a stirring and settling tank filter; the upper part of the dryer is connected with a raw material condenser; the stirring settling tank filter and the raw material condenser are connected with the raw material buffer tank; the raw material delivery pump at the bottom of the raw material buffer tank is connected with a feed inlet of the low-temperature complexing aluminum-removing inlet-outlet heat exchanger; the low-temperature complexing and aluminum removing inlet and outlet heat exchanger feed outlet is connected with the low-temperature cooler inlet; the outlet of the low-temperature cooler is connected with the top of the low-temperature complexing stirring tank; the low-temperature complexing transfer pump at the bottom of the low-temperature complexing stirring tank is connected with a low-temperature complexing stirring tank filter; the bottom of the low-temperature complexing stirring tank filter is connected with a dryer, and the lateral line of the low-temperature complexing and aluminum-removing filter is connected with a discharge inlet of the low-temperature complexing heat exchanger; the outlet of the low-temperature complexing aluminum removal inlet-outlet heat exchanger is connected with the inlet of the liquid-phase aluminum removal preheater; the outlet of the liquid-phase aluminum removal preheater is connected with the top of the liquid-phase aluminum removal tank; the bottom of the liquid phase aluminum removal tank is connected with an evaporation kettle; the top of the evaporation kettle is connected with a gas phase heater; the outlet of the gas phase heater is tightly connected with the bottom of the gas phase aluminum removal column; the top of the gas phase aluminum removal column is connected with a gas phase condenser; the top of the product buffer tank is connected with the outlet of the gas phase condenser, and the bottom of the product buffer tank is connected with a product discharge pump; the inlet of the high-pressure rectifying tower preheater is connected with a product discharge pump, and the outlet of the high-pressure rectifying tower preheater is connected with a high-pressure rectifying tower; the high-pressure rectifying tower comprises a high-pressure rectifying tower condenser and a high-pressure rectifying tower evaporator, and the upper section and the lower section in the tower are random packing or regular packing.
5. The process for realizing the complex removal of aluminum by using chlorosilane by using the device of claim 1 is characterized in that a chlorosilane mixture containing aluminum impurities is fed at the top of a stirring settling tank, is settled and separated, and a mixture at the bottom of the tank is dried by a dryer to separate silicon powder and aluminum slag, and then is condensed by a raw material condenser to enter a raw material buffer tank; the chlorosilane mixture extracted from the side line enters a raw material buffer tank after being filtered and separated by a stirring settling tank filter; the method comprises the following steps of pre-cooling raw materials in a low-temperature complexing and dealuminizing inlet and outlet heat exchanger through low-temperature complexing dealuminizing, cooling the raw materials through a low-temperature cooler, removing aluminum in a low-temperature complexing stirring tank filled with a low-temperature complexing dealuminizing agent, filtering the raw materials through a low-temperature complexing stirring tank filter to remove aluminum chloride waste residues, exchanging heat between a chlorosilane mixture filtered by the low-temperature complexing stirring tank filter and the raw materials conveyed by a raw material buffer tank through the low-temperature complexing dealuminizing inlet and; heating chlorosilane through a liquid-phase dealuminization preheater, and feeding the heated chlorosilane into a liquid-phase dealuminization tank filled with a liquid-phase dealuminization agent for dealuminization; liquid chlorosilane subjected to liquid phase aluminum removal enters a product buffer tank and is transported out through a product discharge pump; and removing aluminum from the chlorosilane mixture through low-temperature complexing and liquid-phase complexing to obtain a high-purity chlorosilane liquid product almost free of aluminum.
6. The process for realizing the complex removal of aluminum by using chlorosilane by using the device of claim 2 is characterized in that a chlorosilane mixture containing aluminum impurities is fed at the top of a stirring settling tank, is settled and separated, and a mixture at the bottom of the tank is dried by a dryer to separate silicon powder and aluminum slag, and then is condensed by a raw material condenser to enter a raw material buffer tank; the chlorosilane mixture extracted from the side line enters a raw material buffer tank after being filtered and separated by a stirring settling tank filter; the method comprises the following steps of pre-cooling raw materials in a low-temperature complexing and dealuminizing inlet and outlet heat exchanger through low-temperature complexing dealuminizing, cooling the raw materials through a low-temperature cooler, removing aluminum in a low-temperature complexing stirring tank filled with a low-temperature complexing dealuminizing agent, filtering the raw materials through a low-temperature complexing stirring tank filter to remove aluminum chloride waste residues, exchanging heat between a chlorosilane mixture filtered by the low-temperature complexing stirring tank filter and the raw materials conveyed by a raw material buffer tank through the low-temperature complexing dealuminizing inlet and; heating chlorosilane through a liquid-phase dealuminization preheater, and feeding the heated chlorosilane into a liquid-phase dealuminization tank filled with a liquid-phase dealuminization agent for dealuminization; evaporating and gasifying liquid chlorosilane subjected to liquid phase dealuminization through an evaporation kettle, heating the liquid chlorosilane through a gas phase heater, introducing the liquid chlorosilane into a gas phase dealuminization column filled with a gas phase complexing dealuminization agent for dealuminization, condensing the gas phase chlorosilane from the top of the gas phase dealuminization column to be in a liquid state through a gas phase condenser, and transporting the liquid chlorosilane to a product buffer tank through a product discharge pump; and (3) performing low-temperature complexing and liquid-phase complexing aluminum removal on the chlorosilane mixture, and performing serial gas-phase complexing aluminum removal on the chlorosilane mixture to obtain a high-purity chlorosilane liquid product almost free of aluminum.
7. The process for realizing the chlorosilane complexing aluminum removal by utilizing the device of claim 3 is characterized in that the chlorosilane complexing aluminum removal process for removing aluminum by high-pressure rectification is connected in series, a chlorosilane mixture containing aluminum impurities is fed at the top of a stirring settling tank, is settled and separated, and a mixture at the bottom of the tank is dried by a drier to separate silicon powder and aluminum slag, and then is condensed by a raw material condenser and enters a raw material buffer tank; the chlorosilane mixture extracted from the side line enters a raw material buffer tank after being filtered and separated by a stirring settling tank filter; the method comprises the following steps of pre-cooling raw materials in a low-temperature complexing and dealuminizing inlet and outlet heat exchanger through low-temperature complexing dealuminizing, cooling the raw materials through a low-temperature cooler, removing aluminum in a low-temperature complexing stirring tank filled with a low-temperature complexing dealuminizing agent, filtering the raw materials through a low-temperature complexing stirring tank filter to remove aluminum chloride waste residues, exchanging heat between a chlorosilane mixture filtered by the low-temperature complexing stirring tank filter and the raw materials conveyed by a raw material buffer tank through the low-temperature complexing dealuminizing inlet and; heating chlorosilane through a liquid-phase dealuminization preheater, and feeding the heated chlorosilane into a liquid-phase dealuminization tank filled with a liquid-phase dealuminization agent for dealuminization; liquid chlorosilane subjected to liquid phase dealuminization is sent to a product buffer tank, chlorosilane in the tank is conveyed to a high-pressure rectifying tower preheater through a product discharge pump and heated, then the liquid chlorosilane is introduced into a high-pressure rectifying tower for high-pressure rectifying dealuminization, finally, an aluminum-containing high-boiling-point substance is separated from the bottom of an evaporator of the high-pressure rectifying tower, and after the purified chlorosilane is condensed and liquefied by a condenser of the high-pressure rectifying tower, part of the purified chlorosilane is extracted to obtain a high-purity chlorosilane liquid product subjected to dealuminization; and (3) performing low-temperature complexing and liquid-phase complexing aluminum removal on the chlorosilane mixture, and performing high-pressure rectification aluminum removal on the chlorosilane mixture to obtain a high-purity chlorosilane liquid product almost free of aluminum.
8. The process for realizing the complex aluminum removal of chlorosilane by utilizing the device of claim 4 is characterized in that the process for simultaneously carrying out the gas phase complex aluminum removal and the high-pressure rectification aluminum removal is connected in series, a chlorosilane mixture containing aluminum impurities is fed at the top of a stirring settling tank, is settled and separated, and is dried and separated by a drier at the bottom of the tank to obtain silicon powder and aluminum slag which are condensed by a raw material condenser and enter a raw material buffer tank; the chlorosilane mixture extracted from the side line enters a raw material buffer tank after being filtered and separated by a stirring settling tank filter; the raw materials are pre-cooled in a heat exchanger through low-temperature complexing aluminum removal, and then cooled through a low-temperature cooler to enter a low-temperature complexing stirring tank filled with a low-temperature complexing aluminum removal agent for aluminum removal; filtering and removing aluminum chloride waste residues through a low-temperature complexing stirring tank filter, wherein a chlorosilane mixture filtered by the low-temperature complexing stirring tank filter and a raw material conveyed by a raw material buffer tank are subjected to low-temperature complexing aluminum removal to exchange heat in a heat exchanger, and precooling the raw material; heating chlorosilane through a liquid-phase dealuminization preheater, and feeding the heated chlorosilane into a liquid-phase dealuminization tank filled with a liquid-phase dealuminization agent for dealuminization; evaporating and gasifying liquid chlorosilane subjected to liquid phase dealuminization through an evaporation kettle, heating the liquid chlorosilane through a gas phase heater, introducing the liquid chlorosilane into a gas phase dealuminization column filled with a gas phase complexing dealuminization agent for dealuminization, and condensing the gas phase chlorosilane discharged from the top of the gas phase dealuminization column to be in a liquid state through a gas phase condenser to a product buffer tank; and (3) conveying the condensed chlorosilane to a high-pressure rectifying tower preheater through a product discharge pump, heating, introducing into a high-pressure rectifying tower for high-pressure rectification and aluminum removal, finally separating an aluminum-containing high-boiling-point substance from the bottom of an evaporator of the high-pressure rectifying tower, and condensing and liquefying the purified chlorosilane through a condenser of the high-pressure rectifying tower to obtain a high-purity chlorosilane liquid product after aluminum removal.
9. The method of claims 5 to 8, wherein when the equipment is in operation, a low-temperature complexing and aluminum removing agent is filled in a low-temperature complexing stirring tank; filling a liquid phase complexing aluminum removing agent in the liquid phase aluminum removing tank; filling a gas phase complexing aluminum removing agent in the gas phase aluminum removing column; and the aluminum removing agents are required to be replaced periodically; wherein the filling amount of the low-temperature complexing aluminum remover and the liquid-phase complexing aluminum remover is 40-50% of the volume of the tank; the filling height of the gas phase aluminum removing agent is 70-80% of the height of the adsorption column; the low-temperature complexing and liquid-phase complexing aluminum removing agent adopts alkali metal, alkaline earth metal salt or a compound thereof, Lewis base containing nitrogen, oxygen, sulfur and phosphorus or a compound thereof, or a mixture of the above substances, preferably lithium chloride, sodium chloride, potassium chloride and amine compounds; the gas-phase complexing aluminum remover adopts alkali metal, alkaline earth metal salt or a compound thereof loaded by a porous material, and Lewis base containing nitrogen, oxygen, sulfur and phosphorus or a compound thereof loaded by the porous material, preferably lithium chloride, sodium chloride, potassium chloride and amine compounds loaded by the porous material; the gas-phase aluminum remover carrier is active carbon or active alumina material with a porous structure, and the loading amount is 5-15% of the mass of the carrier.
10. The method of claims 5 to 8, wherein the low-temperature complexing and aluminum removing inlet and outlet heat exchanger precools the chlorosilane to-10 ℃ to 0 ℃; the precooler continuously cools the precooled chlorosilane to a temperature range of-20 ℃ to-30 ℃; the liquid-phase aluminum removal preheater preheats the chlorosilane mixture subjected to low-temperature complexing aluminum removal to 20-30 ℃; the gas phase heater heats chlorosilane mixed steam from the evaporation kettle to 120-140 ℃; the high-pressure rectifying tower preheater preheats the chlorosilane to 180-220 ℃, and the operating pressure of the high-pressure rectifying tower 2 is 15-35 atm.
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