CN110357915B - System for synthesizing, filtering and purifying silicon ethane - Google Patents
System for synthesizing, filtering and purifying silicon ethane Download PDFInfo
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- CN110357915B CN110357915B CN201810321091.7A CN201810321091A CN110357915B CN 110357915 B CN110357915 B CN 110357915B CN 201810321091 A CN201810321091 A CN 201810321091A CN 110357915 B CN110357915 B CN 110357915B
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- SVXHDONHRAZOCP-UHFFFAOYSA-N ethane;silicon Chemical compound [Si].CC SVXHDONHRAZOCP-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000001914 filtration Methods 0.000 title claims abstract description 28
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 12
- 238000004821 distillation Methods 0.000 claims abstract description 118
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 115
- 229910000077 silane Inorganic materials 0.000 claims abstract description 115
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 55
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 48
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 42
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 29
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 238000000746 purification Methods 0.000 claims abstract description 19
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 18
- 238000007664 blowing Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000002893 slag Substances 0.000 claims abstract description 14
- 238000007599 discharging Methods 0.000 claims abstract description 10
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 9
- 238000009835 boiling Methods 0.000 claims abstract description 9
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 9
- 238000003860 storage Methods 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 18
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 17
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 10
- POXCVKMBBFNXLZ-UHFFFAOYSA-N propane;silicon Chemical compound [Si].CCC POXCVKMBBFNXLZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000011084 recovery Methods 0.000 claims description 10
- 238000005336 cracking Methods 0.000 claims description 8
- 229910001415 sodium ion Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 230000008929 regeneration Effects 0.000 claims description 6
- 238000011069 regeneration method Methods 0.000 claims description 6
- 150000004756 silanes Chemical class 0.000 claims description 6
- 239000003507 refrigerant Substances 0.000 claims description 5
- 229910000831 Steel Inorganic materials 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- NTQGILPNLZZOJH-UHFFFAOYSA-N disilicon Chemical compound [Si]#[Si] NTQGILPNLZZOJH-UHFFFAOYSA-N 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 238000005194 fractionation Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000010959 steel Substances 0.000 claims description 4
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 2
- 239000013589 supplement Substances 0.000 claims 3
- 239000000047 product Substances 0.000 claims 2
- 150000002431 hydrogen Chemical class 0.000 claims 1
- 230000014759 maintenance of location Effects 0.000 claims 1
- 239000011148 porous material Substances 0.000 claims 1
- 238000004064 recycling Methods 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 abstract description 9
- 239000000243 solution Substances 0.000 abstract description 6
- 239000003814 drug Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 description 6
- WQLQSBNFVQMAKD-UHFFFAOYSA-N methane;silicon Chemical compound C.[Si] WQLQSBNFVQMAKD-UHFFFAOYSA-N 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0803—Compounds with Si-C or Si-Si linkages
- C07F7/0805—Compounds with Si-C or Si-Si linkages comprising only Si, C or H atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0803—Compounds with Si-C or Si-Si linkages
- C07F7/0825—Preparations of compounds not comprising Si-Si or Si-cyano linkages
- C07F7/0827—Syntheses with formation of a Si-C bond
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0803—Compounds with Si-C or Si-Si linkages
- C07F7/0825—Preparations of compounds not comprising Si-Si or Si-cyano linkages
- C07F7/0832—Other preparations
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/20—Purification, separation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a system for synthesizing, filtering and purifying silicon ethane, which comprises: the silicon ethane purification system comprises a desiliconized methane distillation tower, a first distillation tower, a second distillation tower and a third distillation tower, wherein the desiliconized methane distillation tower, the first distillation tower, the second distillation tower and the third distillation tower purify and separate silane and silane through the difference of the molecular size and the boiling point of silane, so that the effect of purifying silane with high purity is achieved, micro-nano silicon powder generated by the reaction is filtered by a filter group of the silicon powder filtration treatment system and regenerated by blowing nitrogen in a reverse direction, and a medicine feeding system adds a sodium hydroxide aqueous solution into the filter group, so that the residual micro-nano silicon powder and the sodium hydroxide aqueous solution react to form a sodium silicate solution which is discharged into a slag discharging barrel, and the safety of the slag discharging process is improved.
Description
Technical Field
The invention relates to a silane processing system, in particular to a system capable of promoting high-order silane conversion reaction generation and silicon powder safe filtration processing, and performing silicon ethane synthesis and filtration purification.
Background
Silane (Silane) and Silane (dis) are SEG (specific electronic grade gas), and the main functional application of the SEG is film deposition. The major application industries of silane include LCD panels, solar cells, energy-saving glass, and gas mixing, and the silane is mainly applied in high-quality electronics industries including DRAM, wafer replacement, LED wafers, and silicon-derived chemicals, where the current market price of silane is tens of dollars per kilogram, and the current market price of silane is thousands of dollars per kilogram, because the production technology of the silane product is difficult, and the market supply is not in demand and the market demand is expected to increase more in the future, the price difference is hundreds of times, and because the compactness of silane is excellent and the deposition temperature is lower than that of silane, the silane has a tendency to partially replace silane under the demand of large area, low multi-layer deposition thickness, sub-process, etc. and quality of high-tech products, the market demand has a possibility of explosive expansion, and the known silane conversion reaction process has some disadvantages, and the main reasons are summarized as follows: the reaction selectivity of the silicon ethane is too low, the cost is reduced along with the refinement of the high-purity silicon methane production technology, the problem of environmental influence caused by the storage of reaction slag and the complicated treatment procedure with large energy consumption are solved, for example, silicon powder particles generated by the oxidation reaction of silane due to the operating conditions and the environment of the process procedure can reduce the efficiency of equipment and the production efficiency and increase the frequency of disassembly, cleaning and maintenance, and the danger of combustion in the disassembly and cleaning process can be increased, so the known silicon ethane production process is difficult to meet the economic benefit.
In view of the above, the present inventors have made manufacturing, development and design experiences of related products for many years, and have designed and evaluated the above objects in detail, and finally have obtained a practical invention.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a system for synthesizing, filtering and purifying ethyl silicate, aiming at the above defects existing in the prior art.
The invention provides a system for synthesizing, filtering and purifying silicon ethane, which comprises: a silicon powder filtering treatment system is connected with a deslagging barrel and a dosing system by a filter group, a large amount of micro-nano silicon powder generated by excessive cracking in the process of silane conversion reaction is directly filtered by different aperture precisions of the filter group, the micro-nano silicon powder attached to the filter group is removed in a nitrogen back-blowing regeneration mode and is stored in the deslagging barrel, after the filter group is regenerated by nitrogen back-blowing, a sodium hydroxide aqueous solution is added into the filter group by using the dosing system, so that the residual micro-nano silicon powder and the sodium hydroxide aqueous solution react to form a sodium silicate solution, and then the sodium silicate solution is discharged into the deslagging barrel, and pure water is added after the sodium hydroxide aqueous solution is discharged to clean residual sodium ions attached to the filter group, so that the silane generated by conversion reaction is prevented from being polluted by the sodium ions; a silicon ethane purification system comprises a desiliconized methane distillation tower, a first distillation tower, a second distillation tower, a third distillation tower and a temporary storage tank for silicon ethane which are connected in series in sequence, wherein the desiliconized methane distillation tower, the first distillation tower, the second distillation tower and the third distillation tower purify and separate silicon methane, silicon ethane and high-order silane through the difference of the molecular size and boiling point of silane, so that the purified silicon ethane is stored in the temporary storage tank for silicon ethane, and the separated silicon methane is recovered for carrying out silane conversion reaction again; the silane conversion system comprises a preheater, a converter, a dehydrogenation distillation tower, a silane replenishing barrel and a compressor, wherein the silane replenishing barrel is connected to one end of the preheater and is used as a raw material replenishing source for consumption of silane in a silane conversion reaction process, the other end of the preheater is connected with the converter, silane heated to 400-500 ℃ by the preheater is subjected to a silane conversion reaction in the converter, the silane is partially converted into silane and higher-order silanes, the converter is connected with a filter group of the silicon powder filtration treatment system, silicon powder generated by reaction cracking is intercepted and filtered by the filter group, downstream equipment pipelines cannot be blocked due to accumulation, the outlet of the filter group is connected with the dehydrogenation distillation tower through the compressor, hydrogen which is not condensed and has the minimum molecular weight is separated and removed by the top of the dehydrogenation distillation tower, the bottom of the dehydrogenation distillation tower is connected with the desilication methane distillation tower of the silane purification system, the desilication distillation tower separated silicon methane distillation tower is conveyed into the dehydrogenation distillation tower, and the silane conversion reaction is recycled, and the silane is purified by the high-order silane fractionation system.
The filter group comprises three filters which are connected in series in sequence, and filter elements with filter particle sizes of 25-200 mu m, 1-20 mu m and 0.03-0.8 mu m are arranged in sequence on the three filters. Or the three filters are sequentially provided with filter elements having filter particle diameters of 5 μm, 0.45 μm and 0.1. Mu.m.
The filter core is used for adsorbing and intercepting excessive silicon powder, so that when pressure difference is generated between the inlet and the outlet of the filter due to the fact that the filter core adsorbs and intercepts the excessive silicon powder, the filter can be switched to be used instead, and the filter which is not used is regenerated and cleaned.
The temporary storage tank is also connected with a finished product tank of the silicon ethane, and the finished product tank of the silicon ethane conveys and fills the silicon ethane into a steel cylinder in a condensation vacuum mode for delivery.
Wherein, the bottom of the first distillation tower is connected with a silicon propane distillation system, and the silicon propane and higher-order silanes are purified by the silicon propane distillation system.
Wherein, the silicon ethane purification system is connected with a gas recovery system, and the gas recovery system is used for recovering, circulating and re-purifying the silane gas which does not reach the purity standard.
Wherein, the gas recovery system is respectively connected with a first distillation tower, a second distillation tower and a third distillation tower which is indirectly connected with the temporary storage tank of the silicon ethane to the gas-liquid separation tank of the silicon ethane purification system.
The dehydrogenation distillation tower of the silane conversion system and a liquid nitrogen refrigerant used by a silicon ethane purification system create a required very low temperature environment to distill and separate non-condensed hydrogen and silicon methane with lower boiling points, the liquid nitrogen after heat exchange is vaporized into the very low temperature nitrogen with the temperature close to minus 160 ℃, silicon ethane can be condensed in the first distillation tower, the second distillation tower and the third distillation tower, the condensed silicon ethane is sent to the shell side of the silicon ethane temporary storage tank to be used as cold preserving fluid, and finally the cold preserving fluid is supplied to the filter group to be used as regenerated nitrogen for back-blowing and breaking, so that the liquid nitrogen is effectively utilized for cooling and blowing and breaking.
The first main objective of the present invention is to use silane as a raw material for a silane-to-ethane conversion reaction, heat the silane at a controlled pressure by a preheater of the silane conversion system to raise the temperature, so that the silane is stably thermally cracked and introduced into the converter, so as to promote the reactive hydrogen molecules generated by cracking to perform a reaction synthesis of silane and ethane, filter the solid silicon powder formed by over-cracking by a filter set to intercept, and only the silane gas enters a fractionation and purification device to fractionate and purify, thereby effectively controlling the stability of the silane conversion reaction, and avoiding the storage of reaction-derived slag and the impact of the slag on the environment.
The second main objective of the present invention is to isolate the filter group before the regeneration of the filter group by the reverse blowing of nitrogen, vacuumize the filter group, fill nitrogen to perform flushing and replacement to desorb the silicon powder intercepted by the filter and cracked by the conversion reaction, and manufacture an anaerobic environment, and react the silicon powder with an aqueous solution of sodium hydroxide to produce a water-soluble colloidal substance of sodium silicate in the anaerobic environment, so that after the removal of micro-nano silicon powder by the reverse blowing of nitrogen, the aqueous solution of sodium hydroxide is added to soak, the micro-nano silicon powder is discharged to a slag discharge barrel after being largely reacted, and pure water is added to the filter group to clean the attached residual sodium ions, thereby preventing the silane generated by the conversion reaction from being polluted by the sodium ions, and finally, the filter group can be safely removed, thereby effectively removing the micro-nano silicon powder to maintain the efficiency of the filter, and having the efficacy of improving the safety of the slag discharge process, and preventing the silicon powder from being oxidized and combusted due to being exposed to the atmosphere.
The third main objective of the present invention is that the system for purifying silane comprises a desiliconized methane distillation tower, a first distillation tower, a second distillation tower, a third distillation tower and a temporary storage tank for silane, which are connected in series in sequence, wherein the desiliconized methane distillation tower, the first distillation tower, the second distillation tower and the third distillation tower purify and separate silane, silane and high-order silane through the difference between the molecular size and boiling point of silane, so that purified silane is stored in the temporary storage tank for silane, thereby ensuring that the purity of silane can reach above international standard 4N8+, and further achieving the effect of high-purity purified silane.
Other objects, advantages and novel features of the invention will become apparent from the following detailed description of the invention when considered in conjunction with the drawings.
Drawings
FIG. 1 is a system configuration diagram of a silane conversion system in the present invention.
Fig. 2 is a system configuration diagram of the silicon powder filtration treatment system in the present invention.
Fig. 3 is a system configuration diagram of a system for purifying ethyl silicate in the present invention.
Symbolic description in the drawings:
10. a silicon powder filtering treatment system; 11. a filter group; 111. a filter; 12. a slag discharging barrel; 13. a dosing system; 20. a silico ethane purification system; 21. a desiliconized methane distillation column; 211. a gas-liquid separation tank; 22. a first distillation column; 23. a second distillation column; 24. a third distillation column; 25. a temporary storage tank for the silicon ethane; 26. a silicon ethane finished product tank; 27. a steel cylinder; 28. a gas recovery system; 30. a silane conversion system; 31. a preheater; 32. a converter; 33. a dehydrogenation distillation column; 34. a silicomethane replenishment bucket; 35. a compressor; 40. a silicopropane distillation system.
Detailed Description
For a better understanding and appreciation of the objects, features, and advantages of the invention, reference should be made to the following detailed description taken in conjunction with the accompanying drawings in which:
as shown in fig. 1 and fig. 2, a system for synthesizing and filtering and purifying silicon ethane comprises: a silicon powder filtering processing system 10, a silicon ethane purifying system 20 and a silane converting system 30, the silicon powder filtering processing system 10 connects a row of slag barrel 12 and a medicine adding system 13 with a filter group 11, a large amount of micro-nano silicon powder (Si) generated by excessive cracking in the process of silane converting reaction is directly filtered with different aperture precisions of the filter group 11, and the micro-nano silicon powder attached to the filter group 11 is removed in a nitrogen back blowing regeneration mode and is stored in the slag discharging barrel 12, after the filter group 11 is regenerated by nitrogen back blowing, the medicine adding system 13 is used for adding sodium hydroxide (NaOH) water solution into the filter group 11, so that the residual micro-nano silicon powder and the sodium hydroxide water solution react to form sodium silicate (Na) sodium silicate 2 SiO 3 ) Discharging the solution into the residue discharge barrel 12, and adding pure water (H) after discharging 2 O) washing residual sodium ions (Na) attached to the filter group 11 + ) Avoidance of sodium ion (Na) + ) Contaminating the silane produced by the silane conversion reaction. The reaction formula is as follows:
Si＋2NaOH＋H 2 O－＞Na 2 SiO 3 ＋2H 2 ，
wherein, the filter group 11 includes three filters 111 connected in series in sequence, and the three filters 111 are sequentially provided with filter cores with filter particle sizes of 25 to 200 μm, 1 to 20 μm and 0.03 to 0.8 μm, or the three filters 111 can also be sequentially provided with filter cores with filter particle sizes of 5 μm, 0.45 μm and 0.1 μm, the three filters 111 with different filter particle sizes are provided with arrays, and only one filter group is started at the same time, when the filter 111 intercepts excessive silicon powder and pressure difference is generated at the inlet and outlet of the filter 111, the filter 111 can be switched for replacement, and the filter 111 which is stopped is regenerated and cleaned, and further, because the filter group 11 contains micron-sized and nano-sized silicon powder with different particle sizes, the filter group 11 is regenerated only by reverse blowing nitrogen gas, so that residual silicon powder is always contacted with air and reacts when the filter 111 is disassembledThe present invention overcomes the above-mentioned disadvantages by a unique technique, in which the main body of the filter group 11 is isolated and vacuumized before the filter 111 is regenerated by blowing nitrogen gas back, and nitrogen gas is injected to perform flushing and replacement to desorb the silicon powder cracked by the conversion reaction intercepted by the filter 111, and to produce an oxygen-free environment, and the silicon powder is reacted with an aqueous solution of sodium hydroxide in the oxygen-free environment to produce water-soluble sodium silicate (Na) which is soluble in water 2 SiO 3 ) The colloidal substance is obtained by removing micro-nano silicon powder by back-blowing nitrogen, soaking in aqueous solution of sodium hydroxide, discharging to residue discharge barrel 12 after the micro-nano silicon powder is reacted, and adding pure water to filter 111 for cleaning residual sodium ions (Na) + ) Finally, the micro-nano silicon powder can be safely removed, so that the micro-nano silicon powder can be effectively removed to maintain the efficiency of the filter 111, and the safety of the slag removal process is improved, and the silicon powder is prevented from being exposed in the atmosphere and being oxidized and combusted.
As shown in fig. 1 and fig. 3, the system 20 for purifying silane comprises a desiliconized methane distillation tower 21, a first distillation tower 22, a second distillation tower 23, a third distillation tower 24 and a temporary storage tank 25, which are connected in series, wherein the desiliconized methane distillation tower 21, the first distillation tower 22, the second distillation tower 23 and the third distillation tower 24 are used for separating Silane (SiH) from Silane (SiH) through the difference between the molecular size and boiling point of silane 4 ) Silicon ethane (Si) 2 H 6 ) And high-order silane purification and separation, so that purified silicon ethane is stored in the silicon ethane temporary storage tank 25, the separated silicon methane is recovered for silane conversion reaction again, the silicon ethane temporary storage tank 25 is also connected with a silicon ethane finished product tank 26, the silicon ethane finished product tank 26 conveys and fills the silicon ethane into a steel cylinder 27 in a condensation vacuum mode for shipment, the bottom of the first distillation tower 22 is connected with a silicon propane distillation system 40, and the silicon propane distillation system 40 purifies silicon propane (Si propane) to obtain silicon propane 3 H 8 ) And higher order silanes. The system 20 is connected to a gas recovery system 28, and the gas recovery system 28 recovers and re-purifies the silane gas which has not reached the purity standard, and the gas recovery systems 28 are respectively connected to the system 28A first distillation tower 22, a second distillation tower 23 and a third distillation tower 24 indirectly connected with a temporary storage tank 25 for ethyl silicate to a gas-liquid separation tank 211 of the system 20, and further, a silane liquid-phase mixed liquid separated by the silane conversion system 30 enters the desiliconized methane distillation tower 21, the desiliconized methane distillation tower 21 carries out heat exchange by using a heating medium with the temperature of 100-140 ℃ so as to completely vaporize the methyl silicate in the silane mixed liquid, and the operating pressure of the desiliconized methane distillation tower 21 is controlled to be 3-10kg/cm 2 (g) Then, the boiling point of the silane is controlled to be-90 ℃ to-50 ℃, the boiling point of the silane is controlled to be 20 ℃ to 70 ℃, the flow of a refrigerant is controlled to keep the temperature of gas phase discharge at the top of the desiliconized methane distillation tower 21 at-80 ℃ to-40 ℃, the silane is separated and removed, the silane is conveyed back to the silane conversion system 30 for conversion reaction circulation again, the first distillation tower 22 is used for separating the silane and higher-order silane, in order to ensure that the material feeding source is stable, liquid phase discharge at the bottom of the desiliconized methane distillation tower 21 is not directly conveyed into the first distillation tower 22 but firstly enters a gas-liquid separation groove 211, then is guided into the first distillation tower 22 through the flow control of the gas-liquid separation groove 211, and the operating pressure of the first distillation tower 22 is 0 to 5kg/cm 2 (g) The temperature is 0 ℃ to 120 ℃, the liquid of the ethyl silicate collected and condensed by distillation is conveyed into the second distillation tower 23, the tower bottom of the second distillation tower 23 is heated by heat medium at 100 ℃ to 140 ℃, the liquid phase ethyl silicate at the tower bottom of the second distillation tower 23 is vaporized, distilled and purified to enter the third distillation tower 24, the second distillation tower 23 and the third distillation tower 24 are designed in the same way, the purpose is to ensure that the purity of the ethyl silicate can reach more than international standard 4N8+, and the operating pressure of the two tower tanks is 0 to 5kg/cm 2 (g) The gas phase temperature at the top of the tower is controlled to be between minus 10 ℃ and 25 ℃ by the flow of a refrigerant, the heat exchange is carried out by normal-temperature cooling water at the bottom of the tower, the temperature is controlled to be between 0 ℃ and 30 ℃, and after several stages of distillation and purification, the liquid-phase silicon ethane at the bottom of the third distillation tower 24 is conveyed into the temporary storage tank 25 of the silicon ethane by pressure difference, thereby achieving the effect of refining and purifying the silicon ethane with high purity.
As shown in fig. 1, 2 and 3, the silane conversion system 30 includes a preheater 31, a converter 32, a dehydrogenation distillation tower 33, a silicomethane replenishing barrel 34 and a compressor 35, the silicomethane replenishing barrel 34 is connected to one end of the preheater 31, the silicomethane replenishing barrel 34 is used as a raw material replenishing source for consumption of silicomethane in the silane conversion process, the other end of the preheater 31 is connected to the converter 32, so that the preheater 31 carries out the silane conversion reaction of the silicomethane heated to 400 to 500 ℃ in the converter 32, and the silicomethane is partially converted into the silicoethane and higher-order silanes, and the silane conversion reaction formula is as follows:
nSiH 4 －＞H 2(g) ＋Si (s) ＋SiH 2(g) ＋Si 2 H 6(g) ＋Si 3 H 8(g) ＋Si 4 H 10(g) …，
the converter 32 is connected with the filter group 11 of the silicon powder filtering treatment system 10, so that the silicon powder generated by the reaction cracking is intercepted and filtered by the filter group 11, further, the downstream equipment pipeline cannot be blocked due to accumulation, and in addition, the outlet of the filter group 11 is pressurized to 5-15kg/cm by a compressor 35 2 (g) A hydrogen gas (H) which is connected to the dehydrogenation distillation column 33 and has a minimum molecular weight and is not condensed at the top of the dehydrogenation distillation column 33 2 ) Separating and removing, wherein the bottom of the dehydrogenation distillation tower 33 is connected with the desiliconized methane distillation tower 21 of the system for purifying the silicon ethane 20, so that the silicomethane separated by the desiliconized methane distillation tower 21 is conveyed into the preheater 31 again for conversion reaction circulation, and the silicoethane and the high-order silane separated by the desiliconized methane distillation tower 21 are guided into the subsequent process of the system for purifying the silicon ethane 20 for fractionation and purification.
As shown in fig. 1, 2 and 3, the dehydrogenation distillation tower 33 of the silane conversion system 30 and the liquid nitrogen refrigerant used in the silane purification system 20 create a required very low temperature environment to distill and separate non-condensed hydrogen and silane with lower boiling points, while the liquid nitrogen after heat exchange is vaporized into very low temperature nitrogen with a temperature close to-160 ℃, so that the silane can be condensed in the first distillation tower 22, the second distillation tower 23 and the third distillation tower 24, and then sent to the shell side of the temporary storage tank 25 of the silane as a cold-retention fluid after condensing the silane, and finally supplied to the filter bank 11 for use as nitrogen for back-blowing and regeneration, thereby effectively utilizing the liquid nitrogen to reduce the temperature and blow and clean.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the scope of the invention; therefore, all the equivalent changes and modifications made according to the claims of the present invention should fall within the scope of the present invention.
Claims (6)
1. A system for synthesizing, filtering and purifying silicon ethane is characterized by comprising:
a silicon powder filtering treatment system, wherein the silicon powder filtering treatment system is connected with a slag discharging barrel and a dosing system by a filter group, the filter group comprises three filters which are sequentially connected in series, the three filters are sequentially provided with filter cores with filtering particle sizes of 25-200 mu m, 1-20 mu m and 0.03-0.8 mu m, or the three filters are provided with filter cores with filtering particle sizes of 5 mu m, 0.45 mu m and 0.1 mu m, micro-nano silicon powder generated by over-cracking in the process of silane conversion reaction is directly filtered by different pore sizes of the filter group, the micro-nano silicon powder attached to the filter group is removed in a nitrogen reverse blowing regeneration mode and is stored in the slag discharging barrel, and after the filter group is regenerated by nitrogen reverse blowing, a sodium hydroxide solution is added into the filter group by the dosing system, so that the residual micro-nano silicon powder and the sodium hydroxide solution react to form a sodium silicate solution, then the sodium silicate solution is discharged into the slag discharging barrel, and the residual sodium ions attached to the filter group are cleaned by pure water;
a silicon ethane purification system, which comprises a desiliconized methane distillation tower, a first distillation tower, a second distillation tower, a third distillation tower and a silicon ethane temporary storage tank which are connected in series in sequence, wherein the desiliconized methane distillation tower uses a heating medium at 100-140 ℃ and the operating pressure is controlled at 3-10kg/cm 2 (g) The first distillation tower uses a heating medium at the temperature of 0-120 ℃ and the operating pressure is controlled to be 0-5 kg/cm 2 (g) The second distillation tower uses a heating medium with the temperature of 100-140 ℃ and the operation pressure is controlled to be 0-5 kg/cm 2 (g) And the third distillation tower uses the heat medium and the operation pressure with the same temperature as the second distillation tower to purify and separate the silane, the silane and the high-order silane through the difference of the molecular size and the boiling point of the silane so as to ensure that the silane is pureStoring the silicalite in the temporary storage tank of the silicalite, and recovering the separated silicalite for the silane conversion reaction again; and
a silane conversion system, which comprises a preheater, a converter, a dehydrogenation distillation tower, a silicomethane supplement barrel and a compressor, wherein the silicomethane supplement barrel is connected with one end of the preheater and is used as a raw material supplement source for consumption of the silicomethane in the process of silane conversion reaction, the other end of the preheater is connected with the converter, the silicomethane heated by the preheater to 400-500 ℃ is subjected to silane conversion reaction in the converter, part of the silicomethane is converted into the silicoethane and higher-order silanes, the converter is connected with a filter group of the silicon powder filtration treatment system, the silicon powder generated by reaction and cracking is intercepted and filtered by the filter group, the outlet of the filter group is connected with the dehydrogenation distillation tower through the compressor, and the top of the dehydrogenation distillation tower is used for separating and removing uncondensed hydrogen, the bottom of the dehydrogenation distillation tower is connected with a desiliconized methane distillation tower of the desiliconized methane distillation tower, so that the silane separated by the desiliconized methane distillation tower is conveyed into the preheater again to carry out silane conversion reaction circulation, and the silane and the high-order silane separated by the desiliconized methane distillation tower are introduced into the subsequent process of the desiliconized ethane purification system to carry out fractionation and purification, the dehydrogenation distillation tower of the silane conversion system and a liquid nitrogen refrigerant used by the silane purification system are distilled and separated to not condense hydrogen and silane, the liquid nitrogen after heat exchange is vaporized into nitrogen with the temperature of minus 160 ℃, the silane can be condensed in the first distillation tower, the second distillation tower and the third distillation tower, the condensed silane is sent into the shell side of the temporary storage tank of the silane as a cold retention fluid after the condensation of the silane, and finally the condensed silane is used as nitrogen for back-blown regeneration by the filter group, thereby effectively utilizing the liquid nitrogen to carry out temperature reduction and blowing.
2. The system for synthesizing, filtering and purifying ethyl silicate according to claim 1, wherein three filters with different filtering particle sizes are provided with an array, only one filter is activated at the same time, when the pressure difference between the inlet and the outlet of the filter is different due to the adsorption and the interception of silicon powder by the filter element, the filter can be switched to be used instead, and the filter which is not used is regenerated and cleaned.
3. The system for synthesizing, filtering and purifying ethyl silicate according to claim 1, wherein the ethyl silicate temporary storage tank is further connected with an ethyl silicate finished product tank, and the ethyl silicate is transported and filled into a steel cylinder by the ethyl silicate finished product tank in a condensation vacuum mode for shipment.
4. The system for synthesizing, filtering and purifying silicon ethane as claimed in claim 1, wherein a silicon propane distillation system is connected to the bottom of the first distillation column, and the silicon propane and the high-order silanes are purified by the silicon propane distillation system.
5. The system for synthesizing, filtering and purifying silicon ethane as claimed in claim 1, wherein the silicon ethane purification system is connected with a gas recovery system, and the gas recovery system is used for recovering, recycling and re-purifying the silane gas which does not reach the purity standard.
6. The system for synthesizing, filtering and purifying silicon ethane as claimed in claim 5, wherein the gas recovery system is connected to the first distillation column, the second distillation column and the third distillation column indirectly connected to the temporary storage tank of silicon ethane to the gas-liquid separation tank of the silicon ethane purification system.
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| US20020188146A1 (en) * | 2001-03-30 | 2002-12-12 | Degussa Ag | Apparatus and process for preparing substantially halogen-free trialkoxysilanes |
| CN200964389Y (en) * | 2005-12-09 | 2007-10-24 | 德古萨公司 | Device for continuously preparing halogen-free trialkoxyl silicane |
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