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WO2015170665A1 - Procédé de production de tétraalcoxysilane - Google Patents

Procédé de production de tétraalcoxysilane Download PDF

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Publication number
WO2015170665A1
WO2015170665A1 PCT/JP2015/063015 JP2015063015W WO2015170665A1 WO 2015170665 A1 WO2015170665 A1 WO 2015170665A1 JP 2015063015 W JP2015063015 W JP 2015063015W WO 2015170665 A1 WO2015170665 A1 WO 2015170665A1
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reaction
tetraalkoxysilane
alkali metal
alcohol
produced
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Japanese (ja)
Inventor
訓久 深谷
星集 崔
準哲 崔
堀越　俊雄
佐藤　一彦
弘之 安田
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National Institute of Advanced Industrial Science and Technology AIST
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National Institute of Advanced Industrial Science and Technology AIST
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    • 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
    • C07F7/04—Esters of silicic acids

Definitions

  • the present invention relates to a highly efficient method for producing tetraalkoxysilane, and more particularly to a method for producing tetraalkoxysilane using a metal alkoxide and / or a specific acetal.
  • Tetraalkoxysilane is used as a raw material for producing various silane compounds, organic silicone polymers, various silylating agents, colloidal silica, ceramics and the like.
  • natural silicon dioxide is used as a starting material, mixed with carbon and reduced at high temperature to obtain metallic silicon, which is reacted with chlorine.
  • silicon tetrachloride After manufacturing silicon tetrachloride, a method of further reacting with alcohol is known (see Patent Document 1).
  • Patent Documents 2 and 3 Also known is a production method in which metal silicon and alcohol are directly reacted.
  • An object of the present invention is to provide a method capable of producing tetraalkoxysilane with energy saving and high yield.
  • the present inventors have made it possible to save energy by coexisting a metal alkoxide and / or a specific acetal in a tetraalkoxysilane production method in which alcohol and silicon oxide are reacted. And it discovered that a tetraalkoxysilane could be manufactured with a high yield, and completed this invention.
  • a tetraalkoxysilane production method including a reaction step of reacting an alcohol and silicon oxide, wherein the reaction step satisfies at least one of the following conditions (a) and (b): A method for producing tetraalkoxysilane.
  • A) The reaction is carried out in the presence of a metal alkoxide.
  • B) The reaction is carried out in the presence of an acetal represented by the following general formula (1).
  • R 1 and R 2 each independently represents a hydrogen atom or a hydrocarbon group having 1 to 15 carbon atoms, and R represents a hydrocarbon group having 1 to 15 carbon atoms, provided that R 1 and R 2 Except when both are hydrogen atoms.
  • the reaction is carried out in the presence of an alkali metal compound and / or an alkaline earth metal compound.
  • alkali metal compound according to ⁇ 2> wherein the alkali metal compound is at least one selected from the group consisting of alkali metal hydroxides, alkali metal halides, alkali metal carbonates, and alkali metal bicarbonates.
  • ⁇ 4> The method for producing a tetraalkoxysilane according to any one of ⁇ 1> to ⁇ 3>, wherein the amount (abundance) of the metal alkoxide is 0 to 4 mol relative to 1 mol of the silicon oxide.
  • tetraalkoxysilane can be obtained in high yield using silicon oxide without going through metallic silicon. For this reason, tetraalkoxysilane can be produced at a lower cost, which is more energy efficient than the prior art.
  • the method for producing tetraalkoxysilane which is one embodiment of the present invention (hereinafter sometimes abbreviated as “the production method of the present invention”) is a reaction step for reacting alcohol and silicon oxide (hereinafter abbreviated as “reaction step”).
  • the reaction step satisfies at least one of the following conditions (a) and (b).
  • (A) The reaction is carried out in the presence of a metal alkoxide.
  • the reaction is carried out in the presence of an acetal represented by the following general formula (1).
  • R 1 and R 2 each independently represents a hydrogen atom or a hydrocarbon group having 1 to 15 carbon atoms, and R represents a hydrocarbon group having 1 to 15 carbon atoms, provided that R 1 and R 2 Except when both are hydrogen atoms.
  • the inventors of the present invention focused on a method using alcohol and silicon oxide as a method for producing tetraalkoxysilane that does not go through metal silicon, and as a result of proceeding with the study, in reacting alcohol with silicon oxide, titanium alkoxide and the like It has been found that a tetraalkoxysilane is efficiently produced by the coexistence of a metal alkoxide and / or an acetal represented by the general formula (1).
  • the metal alkoxide and the acetal represented by the general formula (1) serve as a dehydrating agent for appropriately removing water generated by the reaction, and the resulting tetraalkoxy It is thought to suppress the decomposition of silane.
  • metal alkoxide and acetal generate
  • the reaction step is a batch in which alcohol, metal alkoxide (or acetal), and silicon oxide are respectively introduced into a batch reactor and reacted, and then tetraalkoxysilane is recovered.
  • alcohol and metal alkoxide (or acetal) are sequentially charged into a continuous tube reactor, and reacted with silicon oxide to produce tetraalkoxysilane. It means that the reaction may be a continuous reaction that is sequentially recovered.
  • “in the presence” of “in the presence of metal alkoxide” and “in the presence of acetal” means that “metal alkoxide” or “acetal” is added directly to the reactor, and thus “metal alkoxide”
  • metal alkoxide or “acetal” is added directly to the reactor, and thus “metal alkoxide”
  • metal alkoxide” and “acetal” are produced by reacting with alcohol charged into the reactor, and “metal alkoxide” and “acetal” are produced during the reaction process. ”Is also included. Accordingly, it can be said that “metal alkoxide” exists even when tetraethoxytitanium is produced in the reactor by, for example, introducing titanium tetrachloride and ethanol into the reactor.
  • the reaction step is a step of reacting alcohol and silicon oxide, but the type of alcohol is not particularly limited and can be appropriately selected according to the tetraalkoxysilane that is the production purpose.
  • the type of alcohol is not particularly limited and can be appropriately selected according to the tetraalkoxysilane that is the production purpose.
  • tetraalkoxysilane that is the production purpose.
  • the alcohol may be either an aliphatic alcohol or an aromatic alcohol, and the hydrocarbon group in the alcohol may have a branched structure, a cyclic structure, a carbon-carbon unsaturated bond, or the like.
  • Carbon number of alcohol is 1 or more normally, Preferably it is 2 or more, Preferably it is 15 or less, More preferably, it is 10 or less, More preferably, it is 8 or less.
  • Specific alcohols include methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, 2-methyl-1-propanol, 2-methyl-2-propanol, benzyl alcohol, phenol and the like. It is done. Among these, methanol and ethanol are preferable, and methanol is more preferable.
  • tetraalkoxysilane can be produced at a high yield by using the production method of the present invention.
  • the amount of alcohol used is usually more than 0 times, preferably 5 times or more, more preferably 10 times or more, and usually 10,000 times or less, preferably 5000 times the amount of silicon oxide (silicon basis). It is not more than twice, more preferably not more than 3000 times.
  • the reaction step is a step of reacting alcohol and silicon oxide.
  • Silicon oxide means a compound containing silicon atoms (Si) and oxygen atoms (O) as main constituent elements, and silicon monoxide (SiO). , Silicon dioxide (SiO 2 ), or a complex oxide with other metals such as zeolite.
  • Specific examples of silicon oxide include natural minerals such as quartzite, quartz sand, diatomaceous earth, quartz, calcined ash of silicon-containing plants, volcanic ash, silicates, silica gel derived from fumed silica, silica alumina, zeolite Etc.
  • the reaction step is characterized in that (a) the reaction is carried out in the presence of a metal alkoxide, and the alkoxy group of the metal alkoxide preferably has the same hydrocarbon group as the alcohol.
  • a metal alkoxide metals other than alkali metals, alkaline earth metals, lanthanoids, and actinides are preferable. Titanium (Ti), zirconium (Zr), niobium (Nb), hafnium (Hf), tin (Sn) Etc.
  • Specific metal alkoxides include tetramethoxy titanium, tetraethoxy titanium, tetrapropoxy titanium, tetoisopropoxy titanium, tetrabutoxy titanium, tetra-t-butoxy titanium, tetramethoxy zirconium, tetraethoxy zirconium, tetrapropoxy zirconium, tetraiso Propoxyzirconium, tetrabutoxyzirconium, tetra-t-butoxyzirconium, tetramethoxytin, tetraethoxytin, tetrapropoxytin, tetraisopropoxytin, tetrabutoxytin, tetra-t-butoxytin, tetrapentyloxytin, tetrahexyloxytin Tetra-2-ethyl-1-hexyloxytin, dimethyldimethoxytin, dimethyldiethoxytin,
  • a metal alkoxide not only 1 type but in combination of 2 or more types.
  • the amount (abundance) of the metal alkoxide used is usually 0 mol or more, preferably 0.01 mol or more, more preferably 0.1 mol or more, further preferably 0, relative to 1 mol of silicon oxide (in the case of silicon dioxide, based on silicon).
  • tetraalkoxysilane can be produced with higher yield.
  • the reaction step is characterized in that (b) the reaction is carried out in the presence of an acetal represented by the following general formula (1), and the alkoxy group of the acetal has the same hydrocarbon group as the alcohol.
  • an acetal represented by the following general formula (1) and the alkoxy group of the acetal has the same hydrocarbon group as the alcohol.
  • R 1 and R 2 each independently represents a hydrogen atom or a hydrocarbon group having 1 to 15 carbon atoms, and R represents a hydrocarbon group having 1 to 15 carbon atoms, provided that R 1 and R 2 Except when both are hydrogen atoms.
  • the alkoxy group is the same as the alcohol, as shown in the following reaction formula (2), it reacts with water to produce an alcohol, and this alcohol can be used for the reaction.
  • acetals represented by the general formula (1) include benzaldehyde dimethyl acetal, acetaldehyde dimethyl acetal, formaldehyde dimethyl acetal, acetone dimethyl acetal (2,2-dimethoxypropane), acetone diethyl acetal, acetone dibenzyl acetal, diethyl Ketone dimethyl acetal, benzophenone dimethyl acetal, benzyl phenyl ketone dimethyl acetal, cyclohexanone dimethyl acetal, acetophenone dimethyl acetal, 2,2-dimethoxy-2-phenyl acetophenone, 4,4-dimethoxy-2,5-cyclohexadien-1-one acetal And dimethylacetamide diethyl acetal.
  • the acetal represented by the general formula (1) may be used in combination of not only one type but also two or more types.
  • the amount (abundance) of the acetal represented by the general formula (1) is usually 0 mol or more, preferably 0.01 mol or more, more preferably 0, relative to 1 mol of silicon oxide (in the case of silicon dioxide, based on silicon).
  • 0.1 mol or more usually 200 mol or less, preferably 100 mol or less, more preferably 50 mol or less.
  • tetraalkoxysilane can be produced with higher yield.
  • the reaction step is not particularly limited as long as it satisfies at least one of the conditions (a) and (b) described above, but it is preferable to satisfy the following condition (c).
  • (C) The reaction is carried out in the presence of an alkali metal compound and / or an alkaline earth metal compound. In the presence of an alkali metal compound or an alkaline earth metal compound, cleavage of the silicon-oxygen bond of silicon oxide is promoted, and tetraalkoxysilane can be produced in a higher yield.
  • alkali metal and alkaline earth metal in the alkali metal compound and alkaline earth metal compound examples include lithium (Li), sodium (Na), magnesium (Mg), potassium (K), calcium (Ca), cesium (Cs), and the like. Is mentioned.
  • counter ions hydroxides, halides, oxides, carbonates, hydrogen carbonates, alkoxides, silicates, aluminates, phosphates, organic acid salts, sulfates, nitrates and the like can be mentioned. .
  • alkali metal hydroxides, alkali metal halides, alkali metal carbonates, and alkali metal hydrogen carbonates are preferable, and alkali metal hydroxides, alkali metal halides, alkali metal carbonates, and alkali metal hydrogen carbonates are more preferable.
  • alkali metal compound and alkaline earth metal compound include lithium hydroxide, sodium hydroxide, potassium hydroxide, calcium hydroxide, cesium hydroxide, lithium carbonate, sodium carbonate, potassium carbonate, cesium carbonate, sodium fluoride. , Potassium fluoride, cesium fluoride and the like.
  • the total amount used (total abundance) of the alkali metal compound and the alkaline earth metal compound is usually 0 mol or more, preferably 1.0 mol or more, usually 50 mol or less, relative to 1 mol of silicon oxide (in the case of silicon dioxide). Preferably it is 15 mol or less.
  • the reactor for reacting the alcohol and silicon oxide, the operating procedure, the reaction conditions and the like are not particularly limited, and can be appropriately selected according to the purpose.
  • the reactor include a batch reactor (see FIG. 1A) and a continuous tube reactor (see FIG. 1A) as described above.
  • the batch reactor is preferably a pressure resistant reactor such as an autoclave.
  • the operation procedure is as follows. Alcohol, silicon oxide, metal alkoxide, acetal, alkali metal compound, etc. are charged into the reactor, and the inside of the reaction vessel is purged with an atmosphere gas, and then the atmosphere gas is filled. And then heating to the reaction temperature. The filling pressure of the atmospheric gas at 25 ° C.
  • tetraalkoxysilane is preferably 0.1 to 10 MPa. Within the above range, tetraalkoxysilane can be produced with higher yield.
  • atmospheric gas inert gas, such as nitrogen gas and argon gas, a carbon dioxide, etc. are mentioned.
  • silicon oxide, an alkali metal compound or the like is charged into the reactor, and after heating the reaction vessel to the reaction temperature, alcohol, metal alkoxide, acetal or the like as a gas or liquid, A method of continuously charging each is mentioned.
  • a carrier gas may be used for charging the alcohol. Examples of the carrier gas include inert gases such as nitrogen gas and argon gas, and carbon dioxide.
  • the carrier gas supply rate and the like can be appropriately selected according to the size of the reactor, reaction conditions, and the like.
  • the reaction temperature is usually 50 ° C. or higher, preferably 80 ° C. or higher, more preferably 100 ° C. or higher, more preferably 200 ° C. or higher, particularly preferably 220 ° C. or higher, and usually 500 ° C. or lower, preferably 400 ° C. or lower, more Preferably it is 300 degrees C or less, More preferably, it is 280 degrees C or less.
  • the reaction pressure is usually 0.1 MPa or more, preferably 1.0 MPa or more, more preferably 2.0 MPa or more, and usually 20 MPa or less, preferably 15 MPa or less, more preferably 10 MPa or less.
  • the reaction time is usually 1 hour or longer, usually 168 hours or shorter, preferably 120 hours or shorter, more preferably 100 hours or shorter, still more preferably 50 hours or shorter, particularly preferably 24 hours or shorter.
  • tetraalkoxysilane can be produced with higher yield.
  • Example 1 In a 20 mL volume SUS autoclave (manufactured by Nitto Koatsu Co., Ltd.) containing a magnetic stir bar, 0.18 g of silicon dioxide (Fuji Silysia Chemical CARiACT Q-10), 3.0 g of methanol, acetone dimethyl acetal (2, 2-dimethoxypropane) 5.0 g was added. Then, it heated to 242 degreeC, stirring the inside of an autoclave at 1200 rpm, and was made to react for 24 hours. After cooling, the remaining gas was released, and the reaction mixture was analyzed by gas chromatography (Shimadzu Corporation GC-2014ATF / SPL). The yield of tetramethoxysilane based on silicon dioxide was 9%. The results are shown in Table 1.
  • Example 2 In a 20 mL SUS autoclave (manufactured by Nitto Koatsu Co., Ltd.) containing a magnetic stir bar, 0.18 g of silicon dioxide (Fuji Silysia Chemical CARiACT Q-10), 3.0 g of methanol, acetone dimethyl acetal (2,2-dimethoxypropane) ) 5.0 g was added, and argon gas was charged from the cylinder at 25 ° C. at a pressure indicated by a pressure gauge (PGI-50M-MG10, Swagelok FST Co.) so that the inside of the autoclave was 2.0 MPa and stirred for 10 minutes. While holding and sealing.
  • silicon dioxide Fluji Silysia Chemical CARiACT Q-10
  • methanol acetone dimethyl acetal (2,2-dimethoxypropane)
  • Example 3 Except that 2,2-dimethoxypropane was not added to the reaction conditions of Example 1, but 0.02 g of potassium hydroxide and 88% by mass of tetramethoxytitanium (based on 100% by mass of silicon dioxide) were added. In the same manner as in No. 1, tetramethoxysilane was produced. The yield of tetramethoxysilane based on silicon dioxide was 4%. The results are shown in Table 1.
  • Example 4 To the reaction conditions of Example 1, 0.02 g of potassium hydroxide and 88% by mass of tetramethoxytitanium (based on 100% by mass of silicon dioxide) were added in the same manner as in Example 1 to obtain tetramethoxysilane. Manufactured. The yield of tetramethoxysilane based on silicon dioxide was 37%. The results are shown in Table 1.
  • Tetramethoxysilane was produced in the same manner as in Example 1 except that 2,2-dimethoxypropane was not added and 0.02 g of potassium hydroxide was added to the reaction conditions of Example 1. The yield of tetramethoxysilane based on silicon dioxide was less than 1%. The results are shown in Table 1.
  • Example 5 In a 20 mL SUS autoclave (manufactured by Nitto Koatsu Co., Ltd.) containing a magnetic stir bar, 0.09 g of silicon dioxide (Fuji Silysia Chemical CARiACT Q-10), 8.0 g of ethanol, 0.342 g of tetraethoxytitanium, potassium hydroxide 0.0084 g was added and sealed. Then, it heated to 260 degreeC, stirring the inside of an autoclave at 1200 rpm, and was made to react for 24 hours. After cooling, the remaining gas was released, and the reaction mixture was analyzed by gas chromatography (Shimadzu Corporation GC-2014ATF / SPL). The yield of tetraethoxysilane based on silicon dioxide was 15%. The results are shown in Table 2.
  • Tetraethoxysilane was produced in the same manner as in Example 5, except that 0.09 g of Aerosil 300 (manufactured by Nippon Aerosil Co., Ltd.) was used for the reaction conditions of Example 5. The yield of tetraethoxysilane based on silicon dioxide was 19%. The results are shown in Table 2.
  • Tetraethoxysilane was produced in the same manner as in Example 5 except that the amount of potassium hydroxide was 0.042 g with respect to the reaction conditions of Example 5. The yield of tetraethoxysilane based on silicon dioxide was 62%. The results are shown in Table 2.
  • Tetraethoxysilane was produced in the same manner as in Example 5 except that the amount of potassium hydroxide was 0.042 g and the reaction temperature was 220 ° C. with respect to the reaction conditions of Example 5. The yield of tetraethoxysilane based on silicon dioxide was 58%. The results are shown in Table 2.
  • Tetraethoxysilane was produced in the same manner as in Example 5 except that the amount of potassium hydroxide was 0.042 g and the reaction temperature was 240 ° C. with respect to the reaction conditions of Example 5. The yield of tetraethoxysilane based on silicon dioxide was 60%. The results are shown in Table 2.
  • Tetraethoxysilane was produced in the same manner as in Example 5 except that the amount of potassium hydroxide was 0.042 g and the reaction temperature was 280 ° C. with respect to the reaction conditions of Example 5. The yield of tetraethoxysilane based on silicon dioxide was 56%. The results are shown in Table 2.
  • Tetraethoxysilane was produced in the same manner as in Example 5 except that the amount of potassium hydroxide was 0.042 g and the reaction temperature was 300 ° C. with respect to the reaction conditions of Example 5. The yield of tetraethoxysilane based on silicon dioxide was 50%. The results are shown in Table 2.
  • Example 12 For the reaction conditions of Example 5, the amount of tetraethoxytitanium was 0.692 g, the amount of potassium hydroxide was 0.083 g, and the reaction time was 3 hours. Silane was produced. The yield of tetraethoxysilane based on silicon dioxide was 88%. The results are shown in Table 2.
  • Tetraethoxysilane was produced in the same manner as in Example 5 except that 4.8 g of 2,2-diethoxypropane was further added to the reaction conditions of Example 5. The yield of tetraethoxysilane based on silicon dioxide was 8%. The results are shown in Table 2.
  • Tetraethoxysilane was produced in the same manner as in Example 5 except that tetraethoxytitanium was not added and 4.8 g of 2,2-diethoxypropane was added to the reaction conditions of Example 5. The yield of tetraethoxysilane based on silicon dioxide was 15%. The results are shown in Table 2.
  • Example 15 Similar to Example 5, except that the amount of tetraethoxytitanium was 0.692 g, 0.063 g of lithium hydroxide was added instead of potassium hydroxide, and the reaction time was 3 hours with respect to the reaction conditions of Example 5. Tetraethoxysilane was produced by the above procedure. The yield of tetraethoxysilane based on silicon dioxide was 10%. The results are shown in Table 2.
  • Example 16> Similar to Example 5, except that the amount of tetraethoxytitanium was 0.692 g, 0.060 g of sodium hydroxide was added instead of potassium hydroxide, and the reaction time was 3 hours, relative to the reaction conditions of Example 5. Tetraethoxysilane was produced by the above procedure. The yield of tetraethoxysilane based on silicon dioxide was 96%. The results are shown in Table 2.
  • Example 17 Similar to Example 5, except that the amount of tetraethoxytitanium is 0.692 g, 0.249 g of cesium hydroxide is added instead of potassium hydroxide, and the reaction time is 3 hours with respect to the reaction conditions of Example 5. Tetraethoxysilane was produced by the above procedure. The yield of tetraethoxysilane based on silicon dioxide was 75%. The results are shown in Table 2.
  • Example 18 For the reaction conditions of Example 5, the amount of tetraethoxy titanium was 0.692 g, 0.103 g of potassium carbonate was added instead of potassium hydroxide, and the reaction time was 3 hours. Tetraethoxysilane was produced by the operation. The yield of tetraethoxysilane based on silicon dioxide was 96%. The results are shown in Table 2.
  • Example 19 The reaction conditions of Example 5 were the same as those of Example 5, except that the amount of tetraethoxytitanium was 0.692 g, 0.079 g of sodium carbonate was added instead of potassium hydroxide, and the reaction time was 3 hours. Tetraethoxysilane was produced by the operation. The yield of tetraethoxysilane based on silicon dioxide was 37%. The results are shown in Table 2.
  • Example 20> The reaction conditions of Example 5 were the same as Example 5 except that the amount of tetraethoxytitanium was 0.692 g, 0.232 g of cesium carbonate was added instead of potassium hydroxide, and the reaction time was 3 hours. Tetraethoxysilane was produced by the operation. The yield of tetraethoxysilane based on silicon dioxide was 96%. The results are shown in Table 2.
  • Example 21 Similar to Example 5, except that the amount of tetraethoxytitanium was 0.692 g, 0.089 g of potassium fluoride was added instead of potassium hydroxide, and the reaction time was 3 hours with respect to the reaction conditions of Example 5. Tetraethoxysilane was produced by the above procedure. The yield of tetraethoxysilane based on silicon dioxide was 95%. The results are shown in Table 2.
  • Example 22 In a 20 mL SUS autoclave (manufactured by Nitto Koatsu Co., Ltd.) containing a magnetic stir bar, 0.09 g of silicon dioxide (Fuji Silysia Chemical CARiACT Q-10), 12 g of n-butanol, 1.07 g of tetra-n-butoxy titanium, water 0.08 g of potassium oxide was added and sealed. Then, it heated to 260 degreeC, stirring the inside of an autoclave at 1200 rpm, and was made to react for 24 hours. After cooling, the remaining gas was released, and the reaction mixture was analyzed by gas chromatography (Shimadzu Corporation GC-2014ATF / SPL). The yield of tetra n-butoxysilane based on silicon dioxide was 83%. The results are shown in Table 2.
  • Example 23 For the reaction conditions of Example 5, except that tetraethoxyzirconium was used instead of tetraethoxytitanium, 0.814 g, argon atmosphere was used instead of nitrogen atmosphere, and the reaction time was 3 hours. Tetraethoxysilane was produced. The yield of tetraethoxysilane based on silicon dioxide was 2%. The results are shown in Table 2.
  • Example 24 The reaction conditions of Example 5 were the same as those of Example 5, except that 0.955 g of pentaethoxyniobium was used instead of tetraethoxytitanium, an argon atmosphere was used instead of a nitrogen atmosphere, and the reaction time was 3 hours. Tetraethoxysilane was produced. The yield of tetraethoxysilane based on silicon dioxide was 5%. The results are shown in Table 2.
  • tetraalkoxysilane used as a raw material for producing various silane compounds, organic silicone polymers, various silylating agents, colloidal silica, ceramics and the like can be produced with high efficiency.

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Abstract

Le but de la présente invention concerne un procédé de production d'un tétraalcoxysilane à un rendement élevé tout en économisant de l'énergie. Ce procédé de production d'un tétraalcoxysilane comprend une étape de réaction dans laquelle une réaction entre un alcool et de l'oxyde de silicium est induite. Dans le procédé de production d'un tétraalcoxysilane, le tétraalcoxysilane peut être produit à un rendement élevé tout en économisant de l'énergie, par le fait de satisfaire à la condition (a), à savoir que la réaction est induite en présence d'un alcoxyde de métal, et/ou à la condition (b), à savoir que la réaction est induite en présence d'un acétal représenté par la formule générale (1) (dans la formule générale (1) : R1 et R2 représentent chacun indépendamment un atome d'hydrogène ou un groupe hydrocarboné en C1-15, à condition que les cas dans lesquels R1 et R2 représentent tous les deux un atome d'hydrogène soient exclus ; et R représente un groupe hydrocarboné en C1-C15).
PCT/JP2015/063015 2014-05-09 2015-04-30 Procédé de production de tétraalcoxysilane Ceased WO2015170665A1 (fr)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019131672A1 (fr) * 2017-12-27 2019-07-04 国立研究開発法人産業技術総合研究所 Procédé de production de tétraalcoxysilane
WO2019131600A1 (fr) * 2017-12-27 2019-07-04 国立研究開発法人産業技術総合研究所 Procédé de production de tétraalcoxysilane faisant intervenir un oxyde de calcium
WO2019131518A1 (fr) * 2017-12-26 2019-07-04 国立研究開発法人産業技術総合研究所 Procédé de production de tétraalcoxysilane faisant intervenir un agent d'entraînement
JP2019196335A (ja) * 2018-05-10 2019-11-14 国立研究開発法人産業技術総合研究所 有機珪素化合物の製造方法
RU2801799C1 (ru) * 2022-12-05 2023-08-15 Федеральное государственное бюджетное учреждение науки Институт элементоорганических соединений им. А.Н. Несмеянова Российской академии наук (ИНЭОС РАН) Механохимический способ получения алкоксисиланов

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JPS63270689A (ja) * 1987-04-30 1988-11-08 Agency Of Ind Science & Technol シリカからのアルコキシドの直接製造方法
JP2003252879A (ja) * 2001-12-25 2003-09-10 Nippon Shokubai Co Ltd アルコキシシランの製造方法

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JPS63270689A (ja) * 1987-04-30 1988-11-08 Agency Of Ind Science & Technol シリカからのアルコキシドの直接製造方法
JP2003252879A (ja) * 2001-12-25 2003-09-10 Nippon Shokubai Co Ltd アルコキシシランの製造方法

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WO2019131518A1 (fr) * 2017-12-26 2019-07-04 国立研究開発法人産業技術総合研究所 Procédé de production de tétraalcoxysilane faisant intervenir un agent d'entraînement
JPWO2019131518A1 (ja) * 2017-12-26 2020-12-10 国立研究開発法人産業技術総合研究所 助溶媒によるテトラアルコキシシランの製造方法
JP7012382B2 (ja) 2017-12-26 2022-02-14 国立研究開発法人産業技術総合研究所 助溶媒によるテトラアルコキシシランの製造方法
WO2019131672A1 (fr) * 2017-12-27 2019-07-04 国立研究開発法人産業技術総合研究所 Procédé de production de tétraalcoxysilane
WO2019131600A1 (fr) * 2017-12-27 2019-07-04 国立研究開発法人産業技術総合研究所 Procédé de production de tétraalcoxysilane faisant intervenir un oxyde de calcium
JP2019119736A (ja) * 2017-12-27 2019-07-22 国立研究開発法人産業技術総合研究所 テトラアルコキシシランの製造方法
JPWO2019131600A1 (ja) * 2017-12-27 2020-12-24 国立研究開発法人産業技術総合研究所 酸化カルシウムを用いるテトラアルコキシシランの製造方法
US11028106B2 (en) 2017-12-27 2021-06-08 National Institute Of Advanced Industrial Science And Technology Method for producing tetraalkoxysilane
JP7197829B2 (ja) 2017-12-27 2022-12-28 国立研究開発法人産業技術総合研究所 テトラアルコキシシランの製造方法
JP2019196335A (ja) * 2018-05-10 2019-11-14 国立研究開発法人産業技術総合研究所 有機珪素化合物の製造方法
JP7133801B2 (ja) 2018-05-10 2022-09-09 国立研究開発法人産業技術総合研究所 有機珪素化合物の製造方法
RU2801799C1 (ru) * 2022-12-05 2023-08-15 Федеральное государственное бюджетное учреждение науки Институт элементоорганических соединений им. А.Н. Несмеянова Российской академии наук (ИНЭОС РАН) Механохимический способ получения алкоксисиланов

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