CN108774257A - The preparation facilities of tetramethylsilane - Google Patents
The preparation facilities of tetramethylsilane Download PDFInfo
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- CN108774257A CN108774257A CN201810904735.5A CN201810904735A CN108774257A CN 108774257 A CN108774257 A CN 108774257A CN 201810904735 A CN201810904735 A CN 201810904735A CN 108774257 A CN108774257 A CN 108774257A
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- CN
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- Prior art keywords
- reactor
- rectifying column
- tetramethylsilane
- filter
- separation device
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 40
- 238000000926 separation method Methods 0.000 claims abstract description 20
- -1 reactor Chemical compound 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000006096 absorbing agent Substances 0.000 claims description 10
- 239000002808 molecular sieve Substances 0.000 claims description 9
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 9
- 238000005260 corrosion Methods 0.000 claims description 7
- 230000007797 corrosion Effects 0.000 claims description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 4
- 238000012856 packing Methods 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910052573 porcelain Inorganic materials 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052710 silicon Inorganic materials 0.000 abstract description 5
- 239000010703 silicon Substances 0.000 abstract description 5
- 239000000178 monomer Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 9
- 239000012071 phase Substances 0.000 description 8
- 238000001179 sorption measurement Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 239000012535 impurity Substances 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000005046 Chlorosilane Substances 0.000 description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 3
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 3
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- PQDJYEQOELDLCP-UHFFFAOYSA-N trimethylsilane Chemical compound C[SiH](C)C PQDJYEQOELDLCP-UHFFFAOYSA-N 0.000 description 3
- 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 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000005049 silicon tetrachloride Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229940094989 trimethylsilane Drugs 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 101100373011 Drosophila melanogaster wapl gene Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- POFAUXBEMGMSAV-UHFFFAOYSA-N [Si].[Cl] Chemical compound [Si].[Cl] POFAUXBEMGMSAV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- QABCGOSYZHCPGN-UHFFFAOYSA-N chloro(dimethyl)silicon Chemical compound C[Si](C)Cl QABCGOSYZHCPGN-UHFFFAOYSA-N 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- VXWPONVCMVLXBW-UHFFFAOYSA-M magnesium;carbanide;iodide Chemical compound [CH3-].[Mg+2].[I-] VXWPONVCMVLXBW-UHFFFAOYSA-M 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000005055 methyl trichlorosilane Substances 0.000 description 1
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 210000004483 pasc Anatomy 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000010189 synthetic method 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
- 229910052905 tridymite Inorganic materials 0.000 description 1
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
- C07F7/0825—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
- C07F7/20—Purification, separation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
An embodiment of the present invention provides a kind of preparation facilities of tetramethylsilane, including reactor, filter, Liquid liquid Separation device and rectifying column;Wherein, the filter is connected with the reactor, and the Liquid liquid Separation device is connected with the filter, and the rectifying column is connected with the separator.The tetramethylsilane of high-purity can be made using the low-boiling-point substance generated during direct synthesis organic silicon monomer as raw material in the device of an embodiment through the invention.
Description
Technical field
The present invention relates to the preparation facilities of tetramethylsilane, specially a kind of dress preparing tetramethylsilane by purification
It sets.
Background technology
In the production of organosilicon, chloromethanes and metal pasc reaction generate methylchlorosilane, dimethyl two when major product
Chlorosilane, accounts for 80% of total amount or more, meanwhile, it also will produce a large amount of dimethylchlorosilane, dimethyl dichlorosilane (DMCS), methyl trichlorine
Silane, trimethyl silane, tetramethylsilane, silicon tetrachloride, trichlorosilane etc..Related product in these by-products has after refining
Higher added value has very high economic value, such as silicon tetrachloride for manufacturing preform, trichlorine hydrogen after classification recycling
Silicon can be used as the raw material of polysilicon, and trimethyl silane, tetramethylsilane can be used for integrated circuit low-k deposition material
Material etc..Wherein, tetramethylsilane due to the electronegativity of silicon it is relatively low, on four methyl hydrogen atom influence it is smaller, so in core
It can provide stronger signal and a sharp keen absorption peak in magnetic resonance spectrum, and the proton uptake in other general organic compounds
Peak appears at its left side, therefore, usually using tetramethylsilane as nuclear magnetic resonance reference reagent in nuclear magnetic resoance spectrum.
Currently, there are mainly two types of the synthetic methods of tetramethylsilane, first, by tetrachloro silicane or ethyl orthosilicate and methyl
Magnesium iodide reacts to produce.Second is that by chloromethanes and silica flour, react and produce in the presence of copper catalyst, then essence fractionation system
?.However, above two method is prepared in direct synthesis method all suffers from severe reaction conditions, system yield on tetramethylsilane
The problems such as low, high expensive, while being readily incorporated impurity and there are side reactions, increase and further refines difficulty.
And the existing device that tetramethylsilane is prepared by the above method rely primarily on Multistage rectifying tower and absorber into
Row removal of impurities, the introducing of Multistage rectifying tower so that technological process is long, and chlorosilane present in raw material is close with tetramethylsilane boiling point,
Rectifying removal efficiency is low so that unstable product quality.
Invention content
A primary object of the present invention is providing a kind of preparation facilities of tetramethylsilane, including reactor, filter,
Liquid liquid Separation device and rectifying column;Wherein, the filter is connected with the reactor, the Liquid liquid Separation device and the filtering
Device is connected, and the rectifying column is connected with the separator.
According to an embodiment of the present invention, the material of the reactor is stainless steel, and temperature is provided in the reactor
Spend control unit, pressure control components, mixing component and corrosion resisting liner.
According to an embodiment of the present invention, the material of the corrosion resisting liner is polytetrafluoroethylene (PTFE) or ceramics.
According to an embodiment of the present invention, the rectifying column is plate column or packed tower.
According to an embodiment of the present invention, the rectifying column is packed tower.
According to an embodiment of the present invention, the filler of the packed tower is dumped packing.
According to an embodiment of the present invention, the reactor is connected by top with the filter, and the filter is logical
It crosses top with the Liquid liquid Separation device to be connected, the Liquid liquid Separation device is connected by top with the rectifying column, the liquid liquid point
Also it is connected with the bottom of the reactor by bottom from device.
According to an embodiment of the present invention, include the absorbing unit being connected with the rectifying column.
According to an embodiment of the present invention, the rectifying column is connected by tower top with the absorbing unit.
According to an embodiment of the present invention, the absorbing unit includes at least one absorber, is set in the absorber
It is equipped with molecular sieve.
The device of an embodiment through the invention, the low-boiling-point substance with generation during direct synthesis organic silicon monomer are
The tetramethylsilane of high-purity can be made in raw material.
Description of the drawings
Fig. 1 is the structural schematic diagram of the preparation facilities of the tetramethylsilane of an embodiment of the present invention;
Fig. 2 is the flow chart for preparing tetramethylsilane of an embodiment of the present invention.
Specific implementation mode
Embodying the exemplary embodiment of feature of present invention and advantage will describe in detail in the following description.It should be understood that
The present invention can have various variations in different embodiments, neither depart from the scope of the present invention, and theory therein
Bright and diagram inherently is illustrated as being used, rather than to limit the present invention.
An embodiment of the present invention provides a kind of preparation facilities of tetramethylsilane, which can be used for closing with direct method
It is raw material at the low-boiling-point substance generated during organic silicon monomer (especially methylchlorosilane), it is recycled and is refined etc. and is pure
Change handles to prepare tetramethylsilane.
As shown in Figure 1, the preparation facilities of the tetramethylsilane of an embodiment of the present invention, including it is sequentially connected logical reaction
Device 10, filter 20, Liquid liquid Separation device 30 and rectifying column 40.
In an embodiment, temperature control unit, pressure control components and mixing component are provided in reactor 10,
To realize the functions such as temperature control, pressure control, stirring.The material of reactor 10 is stainless steel, such as 316L stainless steels.Due in reactor
Include HCl in 10 products to be reacted, corrosion can be generated to metal, therefore can be in the reaction chamber of reactor 10 and object
Material is in direct contact part setting corrosion resisting liner, and the material of liner can be the corrosion-resistant materials such as polytetrafluoroethylene (PTFE) or ceramics.
In an embodiment, reactor 10 uses magnetic seal, sealing effect good, it can be ensured that No leakage when operation.
Filter 20 is for being filtered the material in system after reaction, in time by the solid in system from material
It removes, avoids that follow-up equipment and pipeline are resulted in blockage and polluted.
In an embodiment, filter 20 is made of filter housing and filter core, is internally provided with the non-dewetting of surface modification
Film, material PTFE, filtering accuracy can be 0.1~2 micron, and the stripping quantity of relevant metal ions is less than 1000ppt so that
Filter 20 has higher flux rate while efficient intercept.
In an embodiment, filter core can be column, and cartridge support layer, guide layer, newel, outline border and end cap are poly-
Propylene material makes it have higher intensity, indeformable under high pressure.
In an embodiment, the setting of Liquid liquid Separation device 30 is provided with liquid inside it there are one import and two outlets
Liquid seperation film mutually detaches grease using the surface tension difference between film and water phase and organic phase (oil phase).Wherein, exist
Two-phase laminated flow is carried out in the continuous flowing of material, process is one-way process, no air-teturning mixed phenomenon, avoids interval and detaches, ensure that
The stable operation of system.
In an embodiment, rectifying column 40 can be plate column or packed tower, such as sieve-plate tower, preferably packed tower,
The filler of packed tower can be metal or nonmetallic regular or dumped packing, preferably dumped packing.
In an embodiment, reactor 10 is connected by top with filter 20, and filter 20 passes through top and liquid liquid
Separator 30 be connected, Liquid liquid Separation device 30 is connected by top with rectifying column 40, Liquid liquid Separation device 30 also by bottom with react
The bottom of device 10 is connected, so that the water phase components of separation can return to reactor 10 and reuse.
In an embodiment, preparation facilities includes the absorbing unit being connected with rectifying column 40, and rectifying column 40 can pass through tower
Top is connected with absorbing unit.
In an embodiment, absorbing unit includes at least one absorber 50, and the filler in absorber 50 can be point
Son sieve.
As shown in Fig. 2, the process that the device of an embodiment prepares tetramethylsilane through the invention includes:Impurity removal reaction
Step, filtration step, water-oil separating step, rectification process step and adsorption step.
Impurity removal reaction step carries out in reactor 10, can be by the chlorine silicon in low-boiling-point substance by reacting for low-boiling-point substance and water
The reactions such as alkane or methylchlorosilane remove, and correlated response formula is as follows.
SiHmCln+H2O—SiO2+ HCl (m+n=4)
In an embodiment, the molar ratio of raw material and water is 1:(1~5), such as 1:2,1:3 etc.;Reaction temperature can be with
It it is 10~60 DEG C, pressure is 0~5bar, and reaction carries out under stirring, can further strengthen two-phase haptoreaction.
Filtration step carries out in filter 20, and after the completion of reaction, the material in reactor 10 is discharged from top, enters
Filter 20 is filtered.By filtration step, the solid in system can be removed from material in time, to avoid to follow-up
Equipment and pipeline result in blockage and pollute.
Water-oil separating step carries out in Liquid liquid Separation device 30, and the water phase components of separation can pass through the bottom of Liquid liquid Separation device 30
Portion's Returning reactor 10 participates in reaction again, thus not only increases the utilization rate of raw material, also can avoid water phase and enters rectifying column
40, and reacted with chlorosilane and generate solid, cause the blocking and pollution of equipment.
The oil phase component of separation enters rectifying column 40 and carries out rectification process step, and the tower top pressure of rectifying column 40 can be
5KPa~100KPa, tower top temperature are 28~49 DEG C, and reflux entry ratio is 2~10, and theoretical cam curve is 40~80.Rectifying column 40
Tower top cooled down using recirculated water, tower reactor is heated using hot water or conduction oil, overhead extraction tetramethylsilane product
It is discharged into absorber 50 with liquid phase state, tower reactor produces high-boiling components, this part high-boiling components carries out recycling and can be used as production silica gel
Raw material, which is the substance high compared with tetramethylsilane boiling point carried secretly in raw material, such as dimethyldichlorosilane, methyl
Trichlorosilane etc..
Adsorption step can be carried out through absorber 50 from the material of 40 overhead extraction of rectifying column, tetramethylsilane is further purified
Alkane.Molecular sieve can be loaded in absorber 50, and by molecular sieve, product is divided according to the difference of molecular diameter in component
From finally obtaining high-purity tetramethylsilane product.
The molecular diameter of tetramethylsilane isTrimethyl silane in impurity isRelevant alkane, alkene
Equimolecular diameter existsWithin, point of impurity composition is carried out to the selection adsorption capacity of different sizes using molecular sieve
From thering is strong adsorption capacity, only molecular diameter to be less than the substance ability of hole diameter polar molecule and unsaturated molecule
Into the inside of molecular sieve bug hole, therefore, hole diameter is selected to existBelow.Molecular sieve can carry out again after adsorption saturation
It is raw to recycle.
In an embodiment, need to be pre-processed before adsorbing using molecular sieve, to remove moisture removal, such as can 90~
Processing is dried to molecular sieve at a temperature of 200 DEG C.To prevent high-temp combustion, can dry under an inert atmosphere, inert gas
Can be nitrogen, argon gas or helium.The ratio of height to diameter of adsorption column is between 2~9, and adsorption temp is between 10~80 DEG C, adsorption column
Inner wall does electrobrightening processing.
Unless limited otherwise, term used herein is the normally understood meaning of those skilled in the art.
Embodiment described in the invention is merely for exemplary purpose, not to limit the scope of the invention,
Those skilled in the art can be made within the scope of the invention various other replacements, changes and improvements, thus, the present invention is not limited to
The above embodiment, and be only defined by the claims.
Claims (10)
1. a kind of preparation facilities of tetramethylsilane, which is characterized in that including:
Reactor;
Filter is connected with the reactor;
Liquid liquid Separation device is connected with the filter;And
Rectifying column is connected with the Liquid liquid Separation device.
2. the apparatus according to claim 1, which is characterized in that the material of the reactor is stainless steel, in the reaction
Temperature control unit, pressure control components, mixing component and corrosion resisting liner are provided in device.
3. the apparatus of claim 2, which is characterized in that the material of the corrosion resisting liner is polytetrafluoroethylene (PTFE) or pottery
Porcelain.
4. the apparatus according to claim 1, which is characterized in that the rectifying column is plate column or packed tower.
5. device according to claim 4, which is characterized in that the rectifying column is packed tower.
6. device according to claim 5, which is characterized in that the filler of the packed tower is dumped packing.
7. device according to any one of claim 1 to 6, which is characterized in that the reactor by top with it is described
Filter is connected, and the filter is connected by top with the Liquid liquid Separation device, and the Liquid liquid Separation device passes through top and institute
It states rectifying column to be connected, the Liquid liquid Separation device is also connected by bottom with the bottom of the reactor.
8. the apparatus according to claim 1, which is characterized in that include the absorbing unit being connected with the rectifying column.
9. device according to claim 8, which is characterized in that the rectifying column passes through tower top and the absorbing unit phase
Even.
10. device according to claim 8, which is characterized in that the absorbing unit includes at least one absorber, in institute
It states and is provided with molecular sieve in absorber.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113214304A (en) * | 2021-04-23 | 2021-08-06 | 洛阳中硅高科技有限公司 | Preparation system and method of tetramethylsilane |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101955496A (en) * | 2009-07-13 | 2011-01-26 | 嘉兴联合化学有限公司 | Process for purifying tetramethylsilane |
CN106966397A (en) * | 2017-04-06 | 2017-07-21 | 洛阳中硅高科技有限公司 | The recovery method of disilicone hexachloride |
-
2018
- 2018-08-09 CN CN201810904735.5A patent/CN108774257A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101955496A (en) * | 2009-07-13 | 2011-01-26 | 嘉兴联合化学有限公司 | Process for purifying tetramethylsilane |
CN106966397A (en) * | 2017-04-06 | 2017-07-21 | 洛阳中硅高科技有限公司 | The recovery method of disilicone hexachloride |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113214304A (en) * | 2021-04-23 | 2021-08-06 | 洛阳中硅高科技有限公司 | Preparation system and method of tetramethylsilane |
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