CN200964389Y - Device for continuously preparing halogen-free trialkoxyl silicane - Google Patents
Device for continuously preparing halogen-free trialkoxyl silicane Download PDFInfo
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- CN200964389Y CN200964389Y CN 200520132155 CN200520132155U CN200964389Y CN 200964389 Y CN200964389 Y CN 200964389Y CN 200520132155 CN200520132155 CN 200520132155 CN 200520132155 U CN200520132155 U CN 200520132155U CN 200964389 Y CN200964389 Y CN 200964389Y
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Abstract
The utility model relates to an equipment for continuously preparing trialkoxy silane without halogen, in particular to an equipment which continuously prepares trialkoxy silane basically without halogen in general formula I, and in particular without chloride, (RO)3SiH(I), wherein Rmeans alkyl which contains one to six carbon atoms. The equipment consists of a main reactor unit (1), at least one of measuring units (2, 3 and 4) used for liquid and/or suspension liquid and connected to the front of the main reactor, at least one of gaseous matter and/or steamed gaseous matter measuring unit (5), and a products processing unit (6) which is connected to the back of the main reactor. The equipment of the utility model can be used continuously and beneficially in trialkoxy silane basically without halogen in general formula I, when the reaction of silicon and alcohols achieves in the inert solvent under the condition that at least one existing copper organic compound is used as catalyst.
Description
Technical field
The present invention relates to a kind of specific installation for preparing the trialkoxy silane of general formula I
(RO)
3SiH (I)，
R is the alkyl that contains 1-6 carbon atom in the formula, this trialkoxy silane be in the presence of copper containing catalyst in inert solvent prepared in reaction by silicon and alcohols.
Background technology
Own notice of invitation body hydrogen organoalkoxysilane such as Trimethoxy silane or triethoxyl silane are one group of important key compound in the organosilicon chemistry.
Can obtain various functional organic hydride compounds such as alkylalkoxy silane, aminoalkyl group organoalkoxysilane, haloalkylalkoxysilan, vinyl alkoxy silane, epoxy alkyl organoalkoxysilane through Si-H functional group by means of hydrosilylation.These compounds have very wide Application Areas.
Base catalysis disproportionation through the hydrogen organoalkoxysilane can obtain high-purity single silane.This list silane for example can be applicable to semi-conductor industry.
Be by preparing hydrogen organoalkoxysilane such as triethoxyl silane (TEOS) and Trimethoxy silane (TMOS) with technical scale now with ethanol or methanol esterification trichlorosilane.Trichlorosilane is by elemental silicon and hcl reaction preparation in industrial-scale production.Comprise two processing steps in the industrial method that is used to prepare TMOS and TEOS, i.e. synthetic the and esterification thereafter of trichlorosilane.Because the famous high chemical corrosion of hydrogenchloride, this two processing step need high facility investment and safeguard the high after-cost of these equipment.In addition, the synthetic generation of trichlorosilane needs with the very high spontaneously inflammable chloride residue of disposing that expends.According to said method Zhi Bei TEOS or TMOS have tangible cl content.Cl content in this product only can drop to the ppm scope by expending very large distillating method.
Many Application Areass constantly increase the demand to not chloride organosilane.And this organosilane can't obtain by existing preparation method.
The method that addresses this problem can be that elemental silicon and alcohols such as methyl alcohol or the catalytic direct reaction of alcoholic acid copper are to form TMOS or TEOS.Although first batch of corresponding patent application can be traced back to 1949 (US 2473260), most of described method is difficult to realize industrial production.Its shortcoming particularly in the preparation of no chlorine used siliceous amount methyl alcohol or ethanol are had very little reactivity, make that the productive rate that reaches by used silicon is extremely low.In addition, the Cu/Si Preparation of catalysts also quite expends, and for example presses the instruction of US 3641007, and copper and silicon carry out sintering and then can make the Cu/Si catalyzer through roll flute under 1050 ℃.Be transformed into organosilane promptly about 5% and be transformed into TMOS using under the methyl alcohol condition under 280 ℃ of temperature of reaction used silicon through reaction only about 8% in 4-5 hour, about 3% is transformed into tetramethoxy-silicane.Because alcoholic acid is than small reactivity, only 6% used silicon is transformed into organosilane under other all identical reaction conditions, and promptly about 5% is transformed into TEOS, and about 1% is transformed into tetraethoxysilane.The chemical reactivity of propyl alcohol and butanols is lower, and the silicon transformation efficiency only is 1.5% and 0.7%.
The method of known a kind of direct synthesization of dimethyl dichlorosilane of copper catalyzed reaction by silicon and methyl chloride is so that be feasible by using chloro-containing reagent with the direct synthesizing organo-silicon alkane of high yield.Obviously this also is fit to the directly synthetic of TEOS and TMOS.In DE-PS 2247872, described selectivity under greater than 90% have industrial significance greater than 70% TEOS productive rate.Here with CuCl as catalyzer.The ethanol that contains 0.17%HF by application is realized additional activation.But fail to obtain free from chloride product as catalyzer owing to use CuCl.The hydrogen fluoride that is added with in this external ethanol has produced etching problem, and also finds trace hydrogen fluoride in product.
The measure of further raising transformation efficiency has been described in European patent 0280517.Here with the used Si powder of the pre-activation of methyl chloride.Use CuCl as catalyzer once more.The TMOS transformation efficiency counts 81% by used silicon, and selectivity is 88%.Reactivity is obviously less in TEOS is synthetic: the silicon transformation efficiency is 60.2% during selectivity 78.4%.This method neither be free from chloride, and its productive rate is little for the industrial application magnetism.
The no chlorine preparation of productive rate greater than the Trimethoxy silane of 80% (by used silicon) described in US-PS 4727173, it is that (purity is 98.5 weight % by methyl alcohol and commercially available Si powder, Fe＜0.5 weight % does not have other activation step) under the effect of copper hydroxide (II), react and prepare as catalyzer.With commercially available through fine grainding Si powder and with Cu (OH)
2The test afterwards of making catalyzer shows, 30% the unsafty productive rate of only having an appointment in TMOS is synthetic.In addition, with the catalytic reacting phase ratio of CuCl, confirm to have higher content of siloxane, this is because Cu (OH)
2Thermolysis becomes CuO and water, and the trialkoxy silane that this water hydrolysis exists causes the alkanol cracking and forms siloxanes.In addition, with commercially available Cu (OH)
2Making catalyzer usually can not the free from chloride TEOS of preparation.
Summary of the invention
Therefore, the object of the present invention is to provide a kind of cheap preparation to be substantially free of the possibility of the trialkoxy silane of chlorine.
This purpose be by of the present invention be used for continuously preparation not the equipment of halogen-containing trialkoxy silane solve, this equipment is characterised in that based on main reactor unit (1), at least one is connected metering unit that is used for liquid and/or suspension (2,3,4) before the main reactor and the unit that is used for the product post-treatment (6) that at least one is used for the metering unit (5) of gaseous state and/or steam attitude material and is connected on the main reactor back.
Be surprised to find that the reaction of silicon and alcohols can be in inert solvent, be preferably in the copper organic compound as in the presence of the catalyzer, carries out especially economically, at this moment can obtain extra high productive rate and extraordinary selectivity in the device that is designed to operation continuously.Should use the silicon of pre-activation of pulverous warp and poor iron.The mantoquita of the new carboxylic acid of preferred especially use is as catalyzer.
Thus, the purpose of this invention is to provide a kind of be used for preparing continuously general formula I be substantially free of halogen, preferably be substantially free of the equipment of the trialkoxy silane of chlorine,
(RO)
3SiH (I)，
R is the alkyl that contains the 1-6 carbon atom in the formula, the alkyl of straight or branched preferably, this equipment based on main reactor unit (1), at least one is connected metering unit that is used for liquid and/or suspension (2,3,4) before the main reactor and the unit that is used for the product post-treatment (6) that at least one is used for the metering unit (5) of gaseous state and/or steam attitude material and is connected on the main reactor back.
Description of drawings
Fig. 1 illustrate the essentially no halogen that is used for preparing continuously general formula I, the preferred embodiment figure of the equipment of free from chloride trialkoxy silane particularly.
Embodiment
Described main reaction unit (1) generally includes heatablely has multistage whipping device (1.1.1) and through the bubble-column reactor (1.1) of the chuck of heat exchanger (1.9) heating.Reflux exchanger (1.2) should be set on the bubble-column reactor top, and this reflux exchanger is used for separating of overhead product and high boiling product.This high boiling product such as inert solvent turn back in the bubble-column reactor through container (1.3) as liquid phase usually again.Overhead product contains trialkoxy silane and excessive pure and mild a spot of solvent usually.Equipment (1.2) can after connect the collection container (1.5) of another condensing equipment (1.4) and overhead product.Should go out bottom product container (1.6) along separate routes from the bottom of bubble-column reactor (1.1), carry out other post-treatment of bottom product, preferably from solvent, separate the silicon of discharging from this container.Bottom product container (1.6) is equipped with whipping device (1.6.1) usually.Through recycle pump (1.7) and heat exchanger (1.8) bottom product is circulated through container (1.6).This bottom product only contains solvent usually in liquid phase, and only contains the silicon of unreacted as solid.
Can add the required raw material of enforcement the inventive method to bubble-column reactor through metering unit (2,3,4) and (5).
Metering unit (2) should comprise basin (2.1), whipping device (2.1.1), inert gas adding (2.5), recycle pump (2.2) that contains feed material (2.3) and the possibility that flows through heat exchanger (2.4) preheating material.Metering unit (2) is preferred for the catalyst solution metering and is input in the main reaction unit (1).
Metering unit (4) should comprise basin (4.1), recycle pump (4.2) that contains feed material (4.2) and the possibility that flows through heat exchanger (4.3) preheating material.Metering unit (4) is preferred for the solvent metering and is input in the main reaction unit (1).
Metering unit (3) should comprise that be suitable for the solid basin (3.1) (as through pneumatic transport), indifferent gas material that contain suitable feed material (3.2) add (3.3) and be used for the isolating filter plant of solid matter (3.4).Metering unit (3) is preferred for the Si powder metering and is input in the main reaction unit (1).
Metering unit (5) should comprise and is used to measure the equipment of gas (5.5) as nitrogen and gaseous feed, or being used for liquid such as methyl alcohol or alcoholic acid is stored the equipment of (5.1) and metering thereafter, described liquid for example also can enter gas phase or liquid phase by the vaporizer (5.3) through preferably being the heat exchanger form.Metering unit (5) is preferred for the alcohols metering and is input in the main reaction unit (1).
Main reaction unit (1) should after be connected to product post-treatment (6).This post-treatment is made up of the thermal separation process that is used for separated portion usually, as is used for separating from trialkoxy silane the distillation tower (6.1) and the dried distillation tower that high boiling component mainly is a solvent (6.2) that separates of usefulness of unreacted alcohol.The preferred distillation tower of this post-treatment through containing a small amount of stagnant liquid carries out.Also can use the protectiveness post-treatment that short residence time(SRT) is carried out in film-type evaporator, falling-film evaporator and distillation tower and its combination.
For example can send in the process again through measuring apparatus (5) from the alcohol of the unreacted of product post-treatment (6).
Equipment of the present invention can be used for advantageously preparing continuously by the reaction of silicon in the inert solvent that has copper containing catalyst to exist and alcohols general formula I essentially no halogen, preferred free from chloride basically trialkoxy silane
(RO)
3SiH (I)，
R is the alkyl that contains the 1-6 carbon atom in the formula, preferably the alkyl of straight or branched.
Term " basic halogen ", " no chlorine " or " do not have chlorine substantially " trialkoxy silane concerning the professional, mean its content of halogen, halide content, cl content or chloride content usually and all be in halogen, particularly chlorine or the muriatic detection limit scope the i.e. compound of≤5 ppm by weight.
In present device (device), normally a kind of process that gas, solid and liquid composition all participate under the principal reaction condition of the continuous preparation of the trialkoxy silane of general formula I.
Should use thermophore oil as inert solvent, preferred trimethylbenzene isomer mixture, preferred especially MARLOTHERM based on hydrocarbon
S.Usually here as reaction medium, used silicon can be suspended in wherein this inert solvent.
In present device, should use copper compound as catalyzer, this catalyzer preferably is dissolved in the inert solvent or in the used alcohol.Should be with ethanol or methyl alcohol as alcohol.Compare with heterogeneous catalytic reaction, catalyzer preferably has obvious advantage with the reaction that dissolved promptly joins in the reaction medium with the homogeneous phase distribution form usually.Soluble free from chloride basically copper compound can produce particularly advantageous response characteristic in reaction medium.
Should use alkylation copper or alkoxylate copper or copper carboxylate as catalyzer.The copper carboxylate that especially preferably contains 3-9 carbon atom is made catalyzer, and the copper carboxylate that more especially preferably contains 7-9 carbon atom is made catalyzer.Particularly use new carboxylic acid and prepare copper carboxylate.
The copper carboxylate of using as preferred catalyst in present device for example is to be prepared under removal reaction water condition with carboxylic acid by copper hydroxide that is derived from free from chloride basically preparation method's gained and/or cupric oxide.This is used preferably to contain metachemistry calculated amount carboxylic acid such as mol ratio be 1: 2 copper hydroxide and/or cupric oxide, and unreacted carboxylic acid can be reinstated distillation method with reaction water one and removes.For example this reaction can be carried out in rotatory evaporator.The removal of reaction water is preferably by gas enclosure distillation (Schleppdestillation) or by vacuum distilling and should be at 20-180 ℃, preferably 140-180 ℃ of temperature range carried out.This maximum temperature is subject to the thermostability of alkoxyl group copper or copper carboxylate, therefore usually≤280 ℃.Equally also can use nitrogen not inerting and reduction dividing potential drop.
The preferred copper carboxylate of using in present device for example also is dissolved in copper carboxylate in the ethanol such as the solution of its 0.1-20 weight %, and particularly the solution of 2-5 weight % is as catalyzer.So the copper carboxylate of preparation can be described by following stoichiometric composition usually:
Cu (RCOO)
xOH
y, x=1 or 2 wherein, y=0 or 1, x+y=2, R=alkyl, alkenyl, aryl.
The copper carboxylate of using as preferred catalyst in present device also can be prepared by metallic copper and carboxylic acid.At this moment available excessive free carboxy acid prepares.This reaction is preferably carried out under 140-180 ℃.Also can use the burnup thing that contains Si and Cu that produces by the trialkoxy silane for preparing general formula I as the copper source.After the reaction of carrying out copper and carboxylic acid, common filtering insoluble component, and make filtrate not contain excessive acid by distillation as mentioned above.
The Powdered silicon of surperficial oxygen and silicon oxide is removed in preferred use basically in present device, preferred especially its granularity d
90Be 20-1000 μ m, d
50Be 10-800 μ m, preferred d
50Be 20-500 μ m, preferred especially d
50Be 30-200 μ m, more preferred d
50Be 10-100 μ m.The mensuration of this size-grade distribution (d-value) is undertaken by laser diffraction (instrument type: Microtrac-" fullrange analyzer ", Leeds and Northrup company).
Here the iron level of used silicon should be less than 0.1 weight %.For example the productive rate when synthesizing TEOS by the inventive method can be greater than 80% by used silicon, and at this moment the Fe content of used silicon preferably is no more than 0.03 weight %.Compare and see, as long as Fe content is in 0.4 weight % scope in the silicon, then the TEOS productive rate is about 50%.When the trialkoxy silane of synthetic general formula I should be that iron-free carries out basically, and will avoid reaction mixture to contact with iron.But for example in present device, can use glass reactor, glazing reactor, copper reactor, copper facing reactor and have specific characteristic and the work apparatus of comparable surface property and device.
The silicon that is used for the reaction of present device can be by getting with hydrogen fluoride trealment, and at this moment solutions employed preferably contains the HF of 0.1-40 weight %, the HF of preferred especially 0.5-5 weight %.The processing of used silicon should moisture/and or pure medium in and should be at 0-100 ℃, preferred 0-50 ℃, preferred especially 10-40 ℃ and more preferably carry out under 20-30 ℃.
Also can be for reacting used silicon through pre-treatment in the moisture and/or pure medium of pH value＞10.As alkaline medium advantageous applications aqueous sodium hydroxide solution, special is 0.1-50 weight % to NaOH content preferably, and more preferably NaOH content is 0.1-10 weight %.
The activation of Si powder should be carried out in the whipping appts that covers rare gas element such as nitrogen.At least 1 minute usually silicon activatory treatment time, preferred 5 minutes to 1 hour, preferred 15-30 minute especially.Contain NaOH solution in application, when particularly NaOH concentration was higher than the HaOH solution of 1 weight %, the treatment time of silicon should not surpass for 1 quarter.
Silicon through so handling can for example be separated from moisture and/or pure by filtering under the oxygen deprivation condition, and the preferred oxygen deprivation water of water and/or alcohols particular methanol or washing with alcohol are operated under the oxygen deprivation condition then equally.For example the residual fluorine content through activatory silicon like this is about the detection limit of 50 ppm by weight to fluorine.The silicon of this processing also can carry out drying after washing, preferably in vacuum, particularly preferably under 0-180 ℃ the vacuum as carry out in rotatory evaporator.The drying of this activation silicon also can preferably be carried out under the inerting condition in other industrially drying device such as vane-type drying machine.This Si powder normally can be used after drying.If treated or dry after should activate silicon immediately and be suspended in for example MARLOTHERM S
In, then can improve and be beneficial to this to the oxygen storage property and the operability of responsive powder especially.This suspended substance can be directly used in the trialkoxy silane of the inventive method with the preparation general formula I.This suspended substance has much lower oxygen sensitivity usually than exsiccant activated powder.Even contact about 1 hour with air after, the use of this suspended substance can not cause the obvious influence to activity usually.But preferably,, generate the trialkoxy silane of general formula I up to reaction particularly preferably in handling activation silicon in the inert reaction medium that is suitable for reacting at the inert liq of oxygen deprivation.
In the methods of the invention, have the copper organic compound as catalyzer in the presence of in the natural instincts solvent reaction of silicon and alcohols preferred 180-260 ℃, carry out under preferred 200-250 ℃ especially usually in 100-350 ℃.
In addition, in present device, have the copper organic compound as in the presence of the catalyzer in inert solvent the reaction of silicon and alcohols carry out under the preferred especially 1-3bar absolute pressure preferably in the 1-5bar absolute pressure.
When the copper organic compound being arranged silicon and alcohols react in inert solvent in the presence of as catalyzer, this catalyzer also can be metered in reaction process again.This catalyzer for example can be dissolved in the used alcohol of reaction for this reason or be dissolved in after in the used inert solvent of reaction medium and being metered into again.
In present device, have the copper organic compound as catalyzer in the presence of in inert solvent the reaction of silicon and alcohols also should have in the presence of the defoaming, particularly have under the methyl-silicone oil existence and carry out, the viscosity of this methyl-silicone oil is preferably 0.65-1000000mPas.For example can use molecular weight here and be the poly-silicon hydrogen alkane of dimethyl of 162-74000g/mol or corresponding mixture as defoaming.
The preferred online hydrogen analysis of use (1.10) is for example carried out technology controlling and process by means of online thermal conductivity detector (WLD) in present device.This detector preferably is connected on the surplus vapour conduit of bubble-column reactor, particularly preferably in condenser (1.4) before.But also can be in the waste gas duct of product post-treatment (6) back with described hydrogen analytical integration.
Bottom product should be sent to the post-treatment that is used for separate solid by bottom product container (1.6), especially preferably is sent in centrifugal filter or the decanting vessel.Unreacted silicon is discharged through gate equipment (7.2), and other post-treatment that can lead.Solvent and high boiling liquid component are discharged through gate equipment (7.3), and part can be through measuring apparatus (4) recirculation.
Can enter in the process again through metering unit (5) as the unreacted alcohol that comes by product post-treatment (6).
Dissolved copper organic compound only is stable through the long period under above-mentioned reaction conditions usually under certain condition in the reaction medium of described process.Even now, employed copper organic compound still has excellent catalytic activity, extraordinary selectivity and high productive rate in described equipment.In addition, the advantage of this copper catalyst is, under the catalytic activity situation that weaken of the form of being in a liquid state during promptly as homogeneous phase solution, can the plain mode metering be added in the reaction mixture.In addition, described method can be carried out in present device is promptly installed especially economically continuously.The chloride content of the trialkoxy silane of the general formula I for preparing in present device advantageously only is≤3 ppm by weight usually.
Embodiment 1
Continuously synthetic (preparation of trialkoxy silane) of trialkoxy silane
The testing apparatus of the trialkoxy silane of preparation general formula I mainly comprises the equipment of detailed earlier herein continuously.
Carry out in reactor volume is about 250 liters functional identical full scale plant by the activation of the silicon of embodiment 3.At this moment under identical feed molar ratio, use 1% the hydrofluoric acid of silicon, 90kg of about 50kg and the ethanol of 71kg.
Preparation of catalysts is carried out in reactor volume is about 35 liters device.At this moment use the new n-nonanoic acid of about 6.8kg, the Cu (OH) of 1.8kg
2Ethanol with 13.4kg.
This is reflected in 10 liters the steel bubble-plate column being with Cu chuck and Cu member and carries out.The multistage internal diameter that whisks the bubble-plate column of device is housed is about 0.2m, and be furnished with and add tower and the partial reflux condenser of building.Surplus vapour is through condensation and then send into rectifying.Alcohol enters bubble-plate column through evaporation and the gas distributor at the bottom of tower.This gas distributor is designed to have the ring nozzle of downward boring.
For beginning reaction, will activate silicon (d
V50Be about 15 μ m) and solvent be added in the reactor as initial batch of material with about 20% outstanding newborn body.Add catalyzer again by about 4% bronze medal of silicon amount.Be similar to intermittent operation, this reactor lockage preface on time is heated to about 200 ℃, is metered into alcohol by about 120mol/h then.This alcohol enters bubble-plate column through evaporation and through the gas distributor at the bottom of tower in preheater.Under normal pressure, temperature is risen to 250 ℃.Reaction process is passed through H
2Generating capacity " online thermal conductivity detector (WLD) " Continuous Tracking in exhaust flow.
Tangible H takes place in the time of about 200 ℃
2Emit this H
2Emitting with the temperature rising increases, and is issued to steady section in constant temperature of reaction.In case H
2Emit decline, then close initial batch of material and can add HF activatory silicon by about 11mol/h continuously.Be metered into copper carboxylate solution by about 200g/h simultaneously as 30 weight % of catalyzer.
Utilize equipment of the present invention for example directly not returning the silicon transformation efficiency of Shi Keda about 65% and about 98% tri-alkoxy selectivity from discharging lock by promptly there being silicon.Space-time yield is the 0.85-1mol/hl trialkoxy silane.
Under the steady running condition, the ethanol of the available about 4kg/h of reaction and mole metering are than being the every mol silicon operation of 6.5mol ethanol.The silicon solids content can fluctuate between 15-30%, and the preferred tunable joint is 20% solids content.The catalyzer metering is counted 3-4g copper by every 100g silicon.Obtain the triethoxyl silane of about 7.5mol/h through the distillate of condensation.
Claims (1)
1. one kind is used for the not equipment of halogen-containing trialkoxy silane of continuously preparation, and this equipment is characterised in that based on main reactor unit (1), at least one is connected metering unit that is used for liquid and/or suspension (2,3,4) before the main reactor and the unit that is used for the product post-treatment (6) that at least one is used for the metering unit (5) of gaseous state and/or steam attitude material and is connected on the main reactor back.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200520132155 CN200964389Y (en) | 2005-12-09 | 2005-12-09 | Device for continuously preparing halogen-free trialkoxyl silicane |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200520132155 CN200964389Y (en) | 2005-12-09 | 2005-12-09 | Device for continuously preparing halogen-free trialkoxyl silicane |
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| Publication Number | Publication Date |
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| CN200964389Y true CN200964389Y (en) | 2007-10-24 |
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ID=38868401
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108383865A (en) * | 2018-03-06 | 2018-08-10 | 宁夏胜蓝化工环保科技有限公司 | The system and method for vapor- phase synthesis Ethoxysilane |
| CN110357915B (en) * | 2018-04-11 | 2023-02-03 | 台湾特品化学股份有限公司 | System for synthesizing, filtering and purifying silicon ethane |
-
2005
- 2005-12-09 CN CN 200520132155 patent/CN200964389Y/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108383865A (en) * | 2018-03-06 | 2018-08-10 | 宁夏胜蓝化工环保科技有限公司 | The system and method for vapor- phase synthesis Ethoxysilane |
| CN108383865B (en) * | 2018-03-06 | 2020-07-17 | 宁夏胜蓝化工环保科技有限公司 | System and method for gas-phase synthesis of ethoxysilane |
| CN110357915B (en) * | 2018-04-11 | 2023-02-03 | 台湾特品化学股份有限公司 | System for synthesizing, filtering and purifying silicon ethane |
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Address after: Dusseldorf Patentee after: DEGUSSA GmbH Address before: Dusseldorf Patentee before: Degussa AG |
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