CN101735257A - Method for synthesizing trimethoxy silane - Google Patents
Method for synthesizing trimethoxy silane Download PDFInfo
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- CN101735257A CN101735257A CN200810235046A CN200810235046A CN101735257A CN 101735257 A CN101735257 A CN 101735257A CN 200810235046 A CN200810235046 A CN 200810235046A CN 200810235046 A CN200810235046 A CN 200810235046A CN 101735257 A CN101735257 A CN 101735257A
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Abstract
The invention relates to a method for synthesizing trimethoxy silane. The trimethoxy silane is prepared by heating metal silicon and methanol at normal pressure under the action of a solvent and a catalyst. The method is characterized in that the catalyst is copper oxide. By using the technical scheme, the method has the advantages that: the utilization rate of silicon powder is over 95 percent; the methanol is completely reacted, so the methanol content in a crude product is less than 1.5 percent; the selectivity of the trimethoxy silane is over 90 percent; and gas entrainment and foam are avoided simultaneously, so that the method greatly improves the production efficiency, reduces the production cost, and also has better economic benefit.
Description
Technical field
The present invention relates to the Synthetic Organic Chemistry technical field, the method for a kind of synthesizing trimethoxy silane of more specifically saying so.
Technical background
Trimethoxy silane (HSi (OMe)
3) both contained hydrolyzable silicon methoxy key, contain active si-h bond again, utilize its hydrolysis properties to can be used as end-capping reagent, the organosilicon end capping that obtains excellent performance solidifies products such as polyethers and polyacrylic ester seal gum; And addition reaction of silicon with hydrogen takes place in si-h bond and a series of vinyl monomer under the katalysis of platinum group catalyst, can obtain various silane coupling agent products, and Trimethoxy silane has important use and is worth, and is very valued in recent years silicone intermediate.Adopt methyl alcohol and silica flour catalyzed reaction synthesizing trimethoxy silane at present both at home and abroad, but this method is more difficult to get the Trimethoxy silane product of highly selective owing to there is the by product tetramethoxy-silicane.The synthesis condition that how to suppress the tetramethoxy-silicane product has become the sector scientific worker's research object, as reaction pressure, temperature, solvent, catalyst activity, feed way and structure of reactor etc.Research in these areas has:
Ritscher; James S., Childress; Thomas E.USP 5,084,590 (1992), under the copper catalyst effect, methyl alcohol and silicon metal successive reaction synthesizing trimethoxy silane.Also optionally in inert solvent or contain at least in many reactive systems of three reactors, and make methyl alcohol flow in the air-flow that contains the silicon metal with the form of steam substantially in the other direction;
Moody; Lawrence G., Childress; Thomas E.Pitrolo; Robert L., Ritscher; James S., Leichliter; Ronald P.USP 4,999,446 (1991), under the copper catalyst effect, methyl alcohol and silicon metal reaction synthesizing trimethoxy silane. also optionally in inert solvent, make Trimethoxy silane-methyl alcohol be recycled, the methyl alcohol turnover ratio is 60%;
Bailey; Donald L., Childress; Thomas E., Ocheltree; Robert L., Ritscher; James S.USP 5,166,384 (1992), use solvent with silicon metal and methyl alcohol synthesizing trimethoxy silane, this method comprises removes the middle dissolved siloxanes that desolvates, and comprise solvent is contacted with the bromine oxygen compound, or selectivity is used basic metal alkyl oxide such as sodium methylate;
Childress; Thomas E., Omietanski; George M., Mendicino; FrankD.USP 4,761, and 492 (1988); Brand; Alexandra, Sterzel; Hans-Josef, USP 6,255, and 514 (2001), a kind of extractive distillation process that from Trimethoxy silane-methyl alcohol miscellany, reclaims methoxy silane.
Though more than improve Trimethoxy silane is synthetic in all its bearings, interest rate and selectivity are still lower.
Summary of the invention
At above-mentioned existing problems, the invention provides a kind of method of synthesizing trimethoxy silane.Method is easy, processing ease, and the Trimethoxy silane selectivity is greater than 90.0%, the silica flour transformation efficiency is tall and big in 95%, and methyl alcohol reacts completely, and methanol content is less than 1.5% in the crude product, and cost is low, the quality product percentage composition is greater than 99.0%, and the yield height has the remarkable economical effect.
In order to reach above purpose, the present invention has adopted following technical scheme: a kind of synthetic method of Trimethoxy silane, and its synthesis step comprises:
A, under normal pressure, Pure Silicon Metal, solvent and catalyzer are added reactor;
B, stirring;
C, in reactor, add methyl alcohol;
D, rectifying separation get Trimethoxy silane,
It is characterized in that: described catalyzer is a cupric oxide.
The present invention is owing to adopted above technical scheme, so have following advantage: the silica flour utilization ratio is tall and big in 95%, methyl alcohol reacts completely in the crude product methanol content less than 1.5%, the Trimethoxy silane selectivity is tall and big in 90%, gas entrainment and foam have been prevented simultaneously, greatly improve production efficiency and reduced production cost, had favorable economic benefit.
Embodiment
Embodiment one:
A kind of method of synthesizing trimethoxy silane, the steps include: A, under normal pressure, Pure Silicon Metal, solvent and catalyzer (cupric oxide) are added reactor, described solvent is one or more in phenyl ether, dibenzyl toluene, hydrogenated terphenyl, the dodecylbenzene etc., the quality feed ratio of silica flour and solvent is 2: 1, and silicon particle size is the 10-60 order; B, stirring, and the air in the logical nitrogen replacement reactive system of methanol feeding mouth; C, in reactor, add methyl alcohol,, methyl alcohol is pumped into reaction from Polycondensation Reactor and Esterification Reactor normal pressure and 150 ℃ (also can be 250 ℃ and following each temperature) as 160,170,180,190,200,210,220,230,240 or 250 ℃; D, rectifying separation get Trimethoxy silane.
Operational instances: be to add the 5000Kg dodecylbenzene in the reactor earlier, start then and stir, rotating speed is transferred to 400r/min, in still, adding 10000Kg silica flour and 10Kg cupric oxide, again with still temperature rise to 230 ℃, stop continuously 36 tons of methyl alcohol being pumped into the reactor internal reaction after the displacement, during beginning the methyl alcohol flow is transferred to 100 kilograms/hour, progressively the methyl alcohol flow is transferred to 500 kilograms/hour then, chromatogram tracking is analyzed, in time regulate the methyl alcohol flow, methanol content in the crude product is controlled at 0.5-2.0%, when dropping to 100 kilograms/hour, the methyl alcohol flow stops charging to the later stage, hydrogen in the logical nitrogen converting system, and add cold thermal oil cooling to the reacting kettle jacketing internal recycle, Trimethoxy silane content is 92.6% in the last crude product, methanol content is 1.3%, obtains 5.1 tons of the tetramethoxy-silicanes of 36.2 tons of 99.3% Trimethoxy silanes and 99.5% after rectifying.
Illustrate: cupric oxide under oxygen free condition with the silica flour Hybrid Heating can react the Red copper oxide silicon alloy.
The present invention adopts cupric oxide to replace conventional cuprous chloride, easier and silica flour react cupro silicon, make reaction more thorough, make silica flour utilization ratio higher (greater than 95%), methyl alcohol reacts completely (methanol content is less than 1.5% in the crude product), Trimethoxy silane selectivity height (greater than 90%), gas entrainment and foam (can not produce the gas as hydrogenchloride) have been prevented simultaneously, greatly improve production efficiency, reduced production cost, had favorable economic benefit.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop in the protection domain of requirement of the present invention.
Claims (4)
1. the synthetic method of a Trimethoxy silane, its synthesis step comprises:
A, under normal pressure, Pure Silicon Metal, solvent and catalyzer are added reactor;
B, stirring;
C, in reactor, add methyl alcohol;
D, rectifying separation get Trimethoxy silane,
It is characterized in that: described catalyzer is a cupric oxide.
2. the synthetic method of a kind of Trimethoxy silane according to claim 1, it is characterized in that: described solvent is one or more in phenyl ether, dibenzyl toluene, hydrogenated terphenyl, the dodecylbenzene etc.
3. the synthetic method of a kind of Trimethoxy silane according to claim 1, it is characterized in that: the mass percent of described silica flour and solvent is 2: 1.
4. the synthetic method of a kind of Trimethoxy silane according to claim 1 is characterized in that: the temperature among the described step D in the reactor is controlled at 150～250 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810235046A CN101735257A (en) | 2008-11-13 | 2008-11-13 | Method for synthesizing trimethoxy silane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810235046A CN101735257A (en) | 2008-11-13 | 2008-11-13 | Method for synthesizing trimethoxy silane |
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| CN101735257A true CN101735257A (en) | 2010-06-16 |
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| CN200810235046A Pending CN101735257A (en) | 2008-11-13 | 2008-11-13 | Method for synthesizing trimethoxy silane |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102532181A (en) * | 2011-12-07 | 2012-07-04 | 诺贝尔（九江）高新材料有限公司 | Alcoholysis process of trimethoxy hydrosilicon |
| CN103204507A (en) * | 2013-04-07 | 2013-07-17 | 李绍光 | Halogen-free silane method for producing solar grade silicon |
| CN104229804A (en) * | 2014-09-15 | 2014-12-24 | 中国科学院过程工程研究所 | Porous silicon material and preparation method of porous silicon material |
| CN107011373A (en) * | 2017-05-16 | 2017-08-04 | 江苏大学 | A kind of CuCl/Cu composite catalysts catalysis methanol reacts the method that direct method prepares trimethoxy silane with silica flour |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10168084A (en) * | 1996-12-06 | 1998-06-23 | Toagosei Co Ltd | Production of alkoxysilane |
| EP1157993A2 (en) * | 2000-05-23 | 2001-11-28 | Basf Aktiengesellschaft | Process for preparing trialkoxysilanes using freshly precipitated CuO as catalyst |
-
2008
- 2008-11-13 CN CN200810235046A patent/CN101735257A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10168084A (en) * | 1996-12-06 | 1998-06-23 | Toagosei Co Ltd | Production of alkoxysilane |
| EP1157993A2 (en) * | 2000-05-23 | 2001-11-28 | Basf Aktiengesellschaft | Process for preparing trialkoxysilanes using freshly precipitated CuO as catalyst |
| US20020010354A1 (en) * | 2000-05-23 | 2002-01-24 | Alexandra Brand | Freshly precipitated CuO as catalyst for the trialkoxysilane synthesis |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102532181A (en) * | 2011-12-07 | 2012-07-04 | 诺贝尔（九江）高新材料有限公司 | Alcoholysis process of trimethoxy hydrosilicon |
| CN102532181B (en) * | 2011-12-07 | 2014-05-28 | 江西晨光新材料有限公司 | Alcoholysis process of trimethoxy hydrosilicon |
| CN103204507A (en) * | 2013-04-07 | 2013-07-17 | 李绍光 | Halogen-free silane method for producing solar grade silicon |
| CN103204507B (en) * | 2013-04-07 | 2018-03-06 | 李绍光 | A kind of Halogen silane thermal decomposition process for producing solar energy level silicon |
| CN104229804A (en) * | 2014-09-15 | 2014-12-24 | 中国科学院过程工程研究所 | Porous silicon material and preparation method of porous silicon material |
| CN107011373A (en) * | 2017-05-16 | 2017-08-04 | 江苏大学 | A kind of CuCl/Cu composite catalysts catalysis methanol reacts the method that direct method prepares trimethoxy silane with silica flour |
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Application publication date: 20100616 |
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