CN109021006A - A kind of pollution-free method for preparing diphenyl diethoxy silane - Google Patents
A kind of pollution-free method for preparing diphenyl diethoxy silane Download PDFInfo
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- CN109021006A CN109021006A CN201811046733.3A CN201811046733A CN109021006A CN 109021006 A CN109021006 A CN 109021006A CN 201811046733 A CN201811046733 A CN 201811046733A CN 109021006 A CN109021006 A CN 109021006A
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- ZZNQQQWFKKTOSD-UHFFFAOYSA-N diethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OCC)(OCC)C1=CC=CC=C1 ZZNQQQWFKKTOSD-UHFFFAOYSA-N 0.000 title claims description 25
- 238000000034 method Methods 0.000 title description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 195
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000012298 atmosphere Substances 0.000 claims abstract description 43
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 11
- 239000011734 sodium Substances 0.000 claims abstract description 11
- 238000010189 synthetic method Methods 0.000 claims abstract description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 9
- GTPDFCLBTFKHNH-UHFFFAOYSA-N chloro(phenyl)silicon Chemical compound Cl[Si]C1=CC=CC=C1 GTPDFCLBTFKHNH-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 72
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 72
- 238000004821 distillation Methods 0.000 claims description 40
- 239000002904 solvent Substances 0.000 claims description 40
- OSXYHAQZDCICNX-UHFFFAOYSA-N dichloro(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](Cl)(Cl)C1=CC=CC=C1 OSXYHAQZDCICNX-UHFFFAOYSA-N 0.000 claims description 38
- 229910052757 nitrogen Inorganic materials 0.000 claims description 36
- 239000003208 petroleum Substances 0.000 claims description 36
- 235000019441 ethanol Nutrition 0.000 claims description 34
- 150000004703 alkoxides Chemical class 0.000 claims description 13
- -1 sodium alkoxide Chemical class 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 2
- LAOYWHMOOCJKMI-UHFFFAOYSA-N chlorobenzene silane Chemical compound [SiH4].C1(=CC=CC=C1)Cl LAOYWHMOOCJKMI-UHFFFAOYSA-N 0.000 claims 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract description 14
- 239000007788 liquid Substances 0.000 abstract description 2
- 238000009938 salting Methods 0.000 abstract description 2
- 238000004090 dissolution Methods 0.000 abstract 1
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical group [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 description 84
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 72
- 238000002360 preparation method Methods 0.000 description 56
- 239000000047 product Substances 0.000 description 51
- 238000006136 alcoholysis reaction Methods 0.000 description 45
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 description 40
- 238000001914 filtration Methods 0.000 description 37
- 239000005054 phenyltrichlorosilane Substances 0.000 description 37
- ORVMIVQULIKXCP-UHFFFAOYSA-N trichloro(phenyl)silane Chemical group Cl[Si](Cl)(Cl)C1=CC=CC=C1 ORVMIVQULIKXCP-UHFFFAOYSA-N 0.000 description 37
- 239000007795 chemical reaction product Substances 0.000 description 36
- AHUXYBVKTIBBJW-UHFFFAOYSA-N dimethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OC)(OC)C1=CC=CC=C1 AHUXYBVKTIBBJW-UHFFFAOYSA-N 0.000 description 18
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 9
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 9
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 8
- 229910000077 silane Inorganic materials 0.000 description 7
- OTEKOJQFKOIXMU-UHFFFAOYSA-N 1,4-bis(trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=C(C(Cl)(Cl)Cl)C=C1 OTEKOJQFKOIXMU-UHFFFAOYSA-N 0.000 description 6
- RCOSUMRTSQULBK-UHFFFAOYSA-N sodium;propan-1-olate Chemical compound [Na+].CCC[O-] RCOSUMRTSQULBK-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- YQGOWXYZDLJBFL-UHFFFAOYSA-N dimethoxysilane Chemical compound CO[SiH2]OC YQGOWXYZDLJBFL-UHFFFAOYSA-N 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- ZXPDYFSTVHQQOI-UHFFFAOYSA-N diethoxysilane Chemical compound CCO[SiH2]OCC ZXPDYFSTVHQQOI-UHFFFAOYSA-N 0.000 description 2
- SLAYMDSSGGBWQB-UHFFFAOYSA-N diphenyl(dipropoxy)silane Chemical compound C=1C=CC=CC=1[Si](OCCC)(OCCC)C1=CC=CC=C1 SLAYMDSSGGBWQB-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- FABOKLHQXVRECE-UHFFFAOYSA-N phenyl(tripropoxy)silane Chemical compound CCCO[Si](OCCC)(OCCC)C1=CC=CC=C1 FABOKLHQXVRECE-UHFFFAOYSA-N 0.000 description 2
- PARWUHTVGZSQPD-UHFFFAOYSA-N phenylsilane Chemical compound [SiH3]C1=CC=CC=C1 PARWUHTVGZSQPD-UHFFFAOYSA-N 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000005046 Chlorosilane Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- SACPKRUZWRIEBW-UHFFFAOYSA-N dipropoxysilane Chemical compound CCCO[SiH2]OCCC SACPKRUZWRIEBW-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- NOKUWSXLHXMAOM-UHFFFAOYSA-N hydroxy(phenyl)silicon Chemical compound O[Si]C1=CC=CC=C1 NOKUWSXLHXMAOM-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000012985 polymerization agent Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 125000001424 substituent group Chemical group 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
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/188—Preparation; Treatments not provided for in C07F7/20 by reactions involving the formation of Si-O linkages
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The present invention relates to a kind of synthetic methods of phenyl alkoxysilane, it is characterized in that first in organic solvent by phenyl chlorosilane dissolution, add alcohol -ol salting liquid, it reacts in an inert atmosphere, after reaction carries out a part, alcohol sodium solution is added again, the reaction was continued, after the completion of reaction, it distills, obtains phenyl alkoxysilane.
Description
Technical field
The present invention relates to a kind of method for preparing alkoxy silane by chlorosilane, especially diphenyl diethoxy silanes
Method.
Background technique
Alkoxy silane is many important materials such as production special polysiloxane, silicon rubber, silicone modified polymers
Raw material.After introducing phenyl in alkoxy silane, the rubber product of preparation can be made still to be able to maintain under ultralow temperature good
Performance, its research and development and application are noticeable at present.
Diphenyl diethoxy silane is the important outer modification of one kind of a kind of organo silane coupling agent and propylene polymerization
Agent, is widely used in the industries such as chemical industry, medicine, dyestuff, aviation, military affairs, and current preparation method mainly includes alcoholysis method, sodium contracting
It is legal etc..
Since prepared by sodium condensation method will use sodium metal, cannot achieve large-scale production, thus present technical grade prepare it is main
It is prepared by phenyl silane alcoholysis, the preparation of phenyl alkoxysilane is mainly prepared by phenyl silane alcoholysis, but logical
To cross alcoholysis and prepare existing larger problem be that yield is often lower, it was also proposed that some improved methods, such as in the reaction plus
Enter acid binding agent, during the reaction shower spray of solvent, neutralizer is added after the reaction was completed in Depressor response etc., and product is repeatedly steamed
The methods of evaporate.But on the whole, the yield of reaction is still unsatisfactory, and reaction cost improves, it is possible to cause safety
Hidden danger.
Therefore, there is an urgent need to the yield of phenyl alkoxysilane product is improved by simply mode at present.
Summary of the invention
Goal of the invention of the invention is to provide a kind of high income, at low cost, is suitable for industrial alkoxy silane
The preparation method of preparation method, especially phenyl alkoxysilane.
The present inventor surprisingly it has been found that when preparing phenyl alkoxysilane, is added corresponding in the course of the research
Sodium alkoxide is especially added portionwise during the reaction, and final product can obtain good yield, and reaction condition is mild, fits
In industrialized production.
The technical solution adopted by the invention is as follows:
A kind of synthetic method of phenyl alkoxysilane, it is characterised in that phenyl chlorosilane is first dissolved in organic solvent
In, alcohol -ol salting liquid is added, is reacted in an inert atmosphere, after reaction carries out a part, alcohol sodium solution is added again, after
Continuous reaction, after the completion of reaction, distillation obtains phenyl alkoxysilane.
Wherein, the phenyl chlorosilane is phenyl trichlorosilane, diphenyl dichlorosilane, and the alcohol is methanol, ethyl alcohol,
The alkoxide is sodium methoxide, and sodium ethoxide, the phenyl alkoxysilane is phenyltrimethoxysila,e, phenyl triethoxy
Silane, dimethoxydiphenylsilane, diphenyl diethoxy silane.
Wherein, the alkoxide -ol total mole number needs the quantity of upper chlorine substituent to determine by phenyl chlorosilane, each chlorine
The alkoxide -ol of the corresponding 0.8~1.5mol of substituent group, the alkoxide -ol of preferably 1~1.5mol, the more preferably alcohol of 1~1.1mol
Salt -ol.
Wherein, the molar ratio of alcohol and alkoxide total amount is (1.5~2.5): 1, preferably (1.8~2.2): 1, more preferably
2.1:1.。
Wherein, the alkoxide amount being added again be alkoxide total amount 40%~60%, phenyl chlorosilane consume 30%~
It is added after 40%.
Wherein, the reaction temperature is 10~80 DEG C, and the preferably reaction time is 4~8 hours.
Organic solvent used in reaction is one or both of n-hexane, petroleum ether, toluene, dimethylbenzene；Further
Preferably, the quality of the organic solvent is the 20%~60% of reaction system gross mass, more preferable 30%~40%.
It needs to be passed through inert gas in reaction to maintain inert atmosphere, which is preferably nitrogen.
In the reaction, water is generated since the HCl of generation can be reacted with methanol, water can promote product to hydrolyze to obtain by-product
Object, therefore reduce the yield of final product.By the present invention in that with alkoxide -ol mixed solution come alcoholysis phenyl chlorosilane, by
In having used alkoxide in this way and can increase the substance of methoxyl group nucleophilie nucleus ability, while alkoxide energy absorbing reaction is generated as catalyst
HCl is converted into alcohol, continuation and silane reaction.In addition, applicant further found that, in the preparation of specific phenyl siloxane, by
Continue to add alkoxide in reaction process, can effectively absorb HCl, avoid the generation of water, further increase the production of final reacting product
Rate.In addition, using the organic solvent of hydrogen chloride solubility very little and being passed through inert gas and excluding chlorination in time when alcoholysis reaction
Hydrogen etc. improves alcoholysis yield to can be reduced side reaction.
The phenyl alkoxysilane synthetic method provided according to the present invention, reaction yield is higher, has reached 90% or more,
And reaction condition is mild, safe operation, is suitable for industrialized production.
Specific embodiment
The present invention is further illustrated below by embodiment.It should be understood that the preparation method of the embodiment of the present invention is only
It is only for illustrating the present invention, rather than limiting the invention, to preparation method of the present invention under concept thereof of the invention
Simple modifications belong to the scope of protection of present invention.Unless otherwise indicated, " % " in the present invention is weight basis.
Embodiment 1: the preparation of phenyltrimethoxysila,e
Petroleum ether is added in three-neck flask as solvent, 1mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 2.1mol methanol and 0.5mol sodium methoxide are added in flask, reacted at 40 DEG C under inert atmosphere that nitrogen, which keeps environment,
After GC monitors phenyl trichlorosilane consumption about 40%, then 0.5mol sodium methoxide is added into reaction system, the reaction was continued, and reaction is altogether
It carries out about 3 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl trimethoxy
Silane, yield 95.85%.
Embodiment 2: the preparation of phenyltrimethoxysila,e
Petroleum ether is added in three-neck flask as solvent, 1mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 2.2mol methanol and 0.5mol sodium methoxide are added in flask, reacted at 40 DEG C under inert atmosphere that nitrogen, which keeps environment,
After GC monitors phenyl trichlorosilane consumption about 30%, then 0.6mol sodium methoxide is added into reaction system, the reaction was continued, and reaction is altogether
It carries out about 3.5 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl trimethoxy
Base silane, yield 95.47%.
Embodiment 3: the preparation of phenyltrimethoxysila,e
Petroleum ether is added in three-neck flask as solvent, 1mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 2.2mol methanol and 0.6mol sodium methoxide are added in flask, reacted at 40 DEG C under inert atmosphere that nitrogen, which keeps environment,
After GC monitors phenyl trichlorosilane consumption about 40%, then 0.4mol sodium methoxide is added into reaction system, the reaction was continued, and reaction is altogether
It carries out about 3 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl trimethoxy
Silane, yield 94.35%.
Embodiment 4: the preparation of phenyltrimethoxysila,e
Petroleum ether is added in three-neck flask as solvent, 3mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 6.1mol methanol and 1.4mol sodium methoxide are added in flask, reacted at 50 DEG C under inert atmosphere that nitrogen, which keeps environment,
After GC monitors phenyl trichlorosilane consumption about 35%, then 1.6mol sodium methoxide is added into reaction system, the reaction was continued, and reaction is altogether
It carries out about 4 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl trimethoxy
Silane, yield 94.56%.
Embodiment 5: the preparation of phenyltrimethoxysila,e
Petroleum ether is added in three-neck flask as solvent, 1mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 2.1mol methanol and 0.5mol sodium methoxide are added in flask, reacted at 40 DEG C under inert atmosphere that nitrogen, which keeps environment,
After GC monitors phenyl trichlorosilane consumption about 20%, then 0.5mol sodium methoxide is added into reaction system, the reaction was continued, and reaction is altogether
It carries out about 4 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl trimethoxy
Silane, yield 91.05%.
Embodiment 6: the preparation of phenyltrimethoxysila,e
Petroleum ether is added in three-neck flask as solvent, 1mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 2.1mol methanol and 0.5mol sodium methoxide are added in flask, reacted at 40 DEG C under inert atmosphere that nitrogen, which keeps environment,
After GC monitors phenyl trichlorosilane consumption about 60%, then 0.6mol sodium methoxide is added into reaction system, the reaction was continued, and reaction is altogether
It carries out about 3 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl trimethoxy
Silane, yield 88.67%.
Embodiment 7: the preparation of phenyltrimethoxysila,e
Petroleum ether is added in three-neck flask as solvent, 1mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 2.1mol methanol and 0.2mol sodium methoxide are added in flask, reacted at 40 DEG C under inert atmosphere that nitrogen, which keeps environment,
After GC monitors phenyl trichlorosilane consumption about 40%, then 0.8mol sodium methoxide is added into reaction system, the reaction was continued, and reaction is altogether
It carries out about 3 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl trimethoxy
Silane, yield 87.5%.
Embodiment 8: the preparation of phenyltrimethoxysila,e
Petroleum ether is added in three-neck flask as solvent, 1mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 2.1mol methanol and 0.8mol sodium methoxide are added in flask, reacted at 40 DEG C under inert atmosphere that nitrogen, which keeps environment,
After GC monitors phenyl trichlorosilane consumption about 40%, then 0.2mol sodium methoxide is added into reaction system, the reaction was continued, and reaction is altogether
It carries out about 3 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl trimethoxy
Silane, yield 84.47%.
Embodiment 9: the preparation of phenyltrimethoxysila,e
Hexamethylene is added in a kettle as solvent, 6.4kg phenyl trichlorosilane is first added, is uniformly mixed, closed
Under inert atmosphere, 2kg methanol and 0.8kg sodium methoxide are added in flask, reacted at 40 DEG C, is carried out 1.5 hours in reaction
Afterwards, then into reaction system 1kg sodium methoxide is added, the reaction was continued, and reaction carries out 4 hours altogether.After completion of the reaction, reaction is collected
Product, filtering, air-distillation obtain alcoholysis product phenyltrimethoxysila,e, yield 92.14%.
Comparative example 1: the preparation of phenyltrimethoxysila,e
In addition to addition 3.1mol methanol, it is added without other than sodium methoxide, is prepared similarly to Example 1, obtain final product,
Yield is 75.4%.
Comparative example 2: the preparation of phenyltrimethoxysila,e
In addition to being prepared other than reaction is initially added into whole methanol and sodium methoxide similarly to Example 1, whole production is obtained
Object, yield 82.55%.
Embodiment 10: the preparation of phenyl triethoxysilane
Petroleum ether is added in three-neck flask as solvent, 1mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 2.1mol ethyl alcohol and 0.5mol sodium ethoxide are added in flask, reacted at 40 DEG C under inert atmosphere that nitrogen, which keeps environment,
After GC monitors phenyl trichlorosilane consumption about 40%, then 0.5mol sodium ethoxide is added into reaction system, the reaction was continued, and reaction is altogether
It carries out about 4 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl triethoxy
Silane, yield 94.65%.
Embodiment 11: the preparation of phenyl triethoxysilane
Petroleum ether is added in three-neck flask as solvent, 1mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 2.2mol ethyl alcohol and 0.5mol sodium ethoxide are added in flask, reacted at 40 DEG C under inert atmosphere that nitrogen, which keeps environment,
After GC monitors phenyl trichlorosilane consumption about 30%, then 0.5mol sodium ethoxide is added into reaction system, the reaction was continued, and reaction is altogether
It carries out about 4 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl triethoxy
Silane, yield 95.1%.
Embodiment 12: the preparation of phenyl triethoxysilane
Petroleum ether is added in three-neck flask as solvent, 1mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 2.1mol ethyl alcohol and 0.6mol sodium ethoxide are added in flask, reacted at 40 DEG C under inert atmosphere that nitrogen, which keeps environment,
After GC monitors phenyl trichlorosilane consumption about 40%, then 0.4mol sodium ethoxide is added into reaction system, the reaction was continued, and reaction is altogether
It carries out about 4 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl triethoxy
Silane, yield 95.35%.
Embodiment 13: the preparation of phenyl triethoxysilane
Petroleum ether is added in three-neck flask as solvent, 3mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 6.4mol ethyl alcohol and 1.2mol sodium ethoxide are added in flask, reacted at 50 DEG C under inert atmosphere that nitrogen, which keeps environment,
After GC monitors phenyl trichlorosilane consumption about 35%, then 1.8mol sodium ethoxide is added into reaction system, the reaction was continued, and reaction is altogether
It carries out about 3 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl triethoxy
Silane, yield 93.56%.
Embodiment 14: the preparation of phenyl triethoxysilane
Petroleum ether is added in three-neck flask as solvent, 1mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 2.1mol ethyl alcohol and 0.5mol sodium ethoxide are added in flask, reacted at 40 DEG C under inert atmosphere that nitrogen, which keeps environment,
After GC monitors phenyl trichlorosilane consumption about 20%, then 0.5mol sodium methoxide is added into reaction system, the reaction was continued, and reaction is altogether
It carries out about 4 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl trimethoxy
Silane, yield 88.4%.
Embodiment 15: the preparation of phenyl triethoxysilane
Petroleum ether is added in three-neck flask as solvent, 1mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 2.1mol ethyl alcohol and 0.5mol sodium ethoxide are added in flask, reacted at 40 DEG C under inert atmosphere that nitrogen, which keeps environment,
After GC monitors phenyl trichlorosilane consumption about 50%, then 0.6mol sodium ethoxide is added into reaction system, the reaction was continued, and reaction is altogether
It carries out about 4 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl trimethoxy
Silane, yield 89.94%.
Embodiment 16: the preparation of phenyl triethoxysilane
Petroleum ether is added in three-neck flask as solvent, 1mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 2.1mol ethyl alcohol and 0.2mol sodium ethoxide are added in flask, reacted at 40 DEG C under inert atmosphere that nitrogen, which keeps environment,
After GC monitors phenyl trichlorosilane consumption about 40%, then 0.8mol sodium ethoxide is added into reaction system, the reaction was continued, and reaction is altogether
It carries out about 3.5 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl trimethoxy
Base silane, yield 87.3%.
Embodiment 17: the preparation of phenyl triethoxysilane
Petroleum ether is added in three-neck flask as solvent, 1mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 2.1mol ethyl alcohol and 0.8mol sodium ethoxide are added in flask, reacted at 40 DEG C under inert atmosphere that nitrogen, which keeps environment,
After GC monitors phenyl trichlorosilane consumption about 40%, then 0.2mol sodium ethoxide is added into reaction system, the reaction was continued, and reaction is altogether
It carries out about 4 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl triethoxy
Silane, yield 83.22%.
Embodiment 18: the preparation of phenyl triethoxysilane
Hexamethylene is added in a kettle as solvent, 6.4kg phenyl trichlorosilane is first added, is uniformly mixed, closed
Under inert atmosphere, 2.8kg ethyl alcohol and 1kg sodium ethoxide are added in flask, reacted at 40 DEG C, after reaction carries out 2 hours,
1.1kg sodium ethoxide is added into reaction system again, the reaction was continued, and reaction carries out 5 hours altogether.After completion of the reaction, reaction is collected
Product, filtering, air-distillation obtain alcoholysis product phenyl triethoxysilane, yield 90.14%.
Comparative example 3: the preparation of phenyl triethoxysilane
In addition to 3.1mol ethyl alcohol is added, it is added without other than sodium ethoxide, is prepared similarly to Example 10, obtain whole production
Object, yield 71.4%.
Comparative example 4: the preparation of phenyl triethoxysilane
In addition to being prepared other than reaction is initially added into whole ethyl alcohol and sodium ethoxide similarly to Example 10, end is obtained
Product, yield 80.1%.
Embodiment 19: the preparation of phenyl tripropoxy silane
Petroleum ether is added in three-neck flask as solvent, 1mol phenyl trichlorosilane is first added, is uniformly mixed, is being passed through
It is that 2mol propyl alcohol and 0.5mol sodium propoxide are added in flask, reacted at 50 DEG C, GC under inert atmosphere that nitrogen, which keeps environment,
Monitor phenyl trichlorosilane consumption about 40% after, then into reaction system be added 0.5mol sodium propoxide, the reaction was continued, reaction altogether into
Row about 3 hours.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product phenyl tripropoxy silicon
Alkane, yield 85.3%.
Comparative example 5: the preparation of phenyl tripropoxy silane
In addition to being prepared other than reaction is initially added into whole propyl alcohol and sodium propoxide similarly to Example 19, end is obtained
Product, yield 81.4%.
Embodiment 20: the preparation of dimethoxydiphenylsilane
Petroleum ether is added in three-neck flask as solvent, 1mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 1.5mol methanol and 0.3mol sodium methoxide are added in flask under inert atmosphere, anti-at 40 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 40%, then 0.3mol sodium methoxide is added into reaction system, the reaction was continued,
Reaction carries out about 3.5 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product hexichol
Base dimethoxysilane, yield 93.77%.
Embodiment 21: the preparation of dimethoxydiphenylsilane
Petroleum ether is added in three-neck flask as solvent, 1mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 1.4mol methanol and 0.3mol sodium methoxide are added in flask under inert atmosphere, anti-at 40 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 30%, then 0.4mol sodium methoxide is added into reaction system, the reaction was continued,
Reaction carries out about 3 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product diphenyl
Dimethoxysilane, yield 93.47%.
Embodiment 22: the preparation of dimethoxydiphenylsilane
Petroleum ether is added in three-neck flask as solvent, 1mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 1.5mol methanol and 0.3mol sodium methoxide are added in flask under inert atmosphere, anti-at 40 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 40%, then 0.4mol sodium methoxide is added into reaction system, the reaction was continued,
Reaction carries out about 4 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product diphenyl
Dimethoxysilane, yield 94.16%.
Embodiment 23: the preparation of dimethoxydiphenylsilane
Petroleum ether is added in three-neck flask as solvent, 3mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 4.6mol methanol and 0.6mol sodium methoxide are added in flask under inert atmosphere, anti-at 50 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 35%, then 0.6mol sodium methoxide is added into reaction system, the reaction was continued,
Reaction carries out about 4.5 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product hexichol
Base dimethoxysilane, yield 93.89%.
Embodiment 24: the preparation of dimethoxydiphenylsilane
Petroleum ether is added in three-neck flask as solvent, 1mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 1.4mol methanol and 0.3mol sodium methoxide are added in flask under inert atmosphere, anti-at 40 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 20%, then 0.3mol sodium methoxide is added into reaction system, the reaction was continued,
Reaction carries out about 3 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product diphenyl
Dimethoxysilane, yield 90.87%.
Embodiment 25: the preparation of dimethoxydiphenylsilane
Petroleum ether is added in three-neck flask as solvent, 1mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 1.5mol methanol and 0.3mol sodium methoxide are added in flask under inert atmosphere, anti-at 40 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 60%, then 0.4mol sodium methoxide is added into reaction system, the reaction was continued,
Reaction carries out about 3.5 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product hexichol
Base dimethoxysilane, yield 87.88%.
Embodiment 26: the preparation of dimethoxydiphenylsilane
Petroleum ether is added in three-neck flask as solvent, 1mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 1.5mol methanol and 0.1mol sodium methoxide are added in flask under inert atmosphere, anti-at 40 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 40%, then 0.5mol sodium methoxide is added into reaction system, the reaction was continued,
Reaction carries out about 3 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product diphenyl
Dimethoxysilane, yield 84.7%.
Embodiment 27: the preparation of dimethoxydiphenylsilane
Petroleum ether is added in three-neck flask as solvent, 1mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 1.6mol methanol and 0.4mol sodium methoxide are added in flask under inert atmosphere, anti-at 40 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 40%, then 0.2mol sodium methoxide is added into reaction system, the reaction was continued,
Reaction carries out about 3 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product diphenyl
Dimethoxysilane, yield 83.21%.
Embodiment 28: the preparation of dimethoxydiphenylsilane
Hexamethylene is added in a kettle as solvent, 7.6kg diphenyl dichlorosilane is first added, is uniformly mixed, close
It closes under inert atmosphere, 1.3kg methanol and 0.5kg sodium methoxide is added in flask, reacted at 40 DEG C, it is small to carry out 2 in reaction
Shi Hou, then 0.6kg sodium methoxide is added into reaction system, the reaction was continued, and reaction carries out 4 hours altogether.After completion of the reaction, it collects
Reaction product, filtering, air-distillation obtain alcoholysis product dimethoxydiphenylsilane, yield 91.22%.
Comparative example 6: the preparation of dimethoxydiphenylsilane
In addition to 3.1mol methanol is added, it is added without other than sodium methoxide, is prepared similarly to Example 20, obtain whole production
Object, yield 78.3%.
Comparative example 7: the preparation of dimethoxydiphenylsilane
In addition to being prepared other than reaction is initially added into whole methanol and sodium methoxide similarly to Example 20, end is obtained
Product, yield 84.21%.
Embodiment 29: the preparation of diphenyl diethoxy silane
Petroleum ether is added in three-neck flask as solvent, 1mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 1.6mol ethyl alcohol and 0.3mol sodium ethoxide are added in flask under inert atmosphere, anti-at 40 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 40%, then 0.3mol sodium ethoxide is added into reaction system, the reaction was continued,
Reaction carries out about 3 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product diphenyl
Diethoxy silane, yield 92.97%.
Embodiment 30: the preparation of diphenyl diethoxy silane
Petroleum ether is added in three-neck flask as solvent, 1mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 1.5mol ethyl alcohol and 0.3mol sodium ethoxide are added in flask under inert atmosphere, anti-at 40 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 30%, then 0.4mol sodium ethoxide is added into reaction system, the reaction was continued,
Reaction carries out about 3.5 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product hexichol
Base diethoxy silane, yield 93.11%.
Embodiment 31: the preparation of diphenyl diethoxy silane
Petroleum ether is added in three-neck flask as solvent, 1mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 1.4mol ethyl alcohol and 0.3mol sodium ethoxide are added in flask under inert atmosphere, anti-at 40 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 40%, then 0.4mol sodium ethoxide is added into reaction system, the reaction was continued,
Reaction carries out about 4 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product diphenyl
Diethoxy silane, yield 93.21%.
Embodiment 32: the preparation of diphenyl diethoxy silane
Petroleum ether is added in three-neck flask as solvent, 3mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 4.5mol ethyl alcohol and 0.6mol sodium ethoxide are added in flask under inert atmosphere, anti-at 50 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 35%, then 0.6mol sodium ethoxide is added into reaction system, the reaction was continued,
Reaction carries out about 4 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product diphenyl
Diethoxy silane, yield 92.89%.
Embodiment 33: the preparation of diphenyl diethoxy silane
Petroleum ether is added in three-neck flask as solvent, 1mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 1.5mol ethyl alcohol and 0.4mol sodium ethoxide are added in flask under inert atmosphere, anti-at 40 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 20%, then 0.3mol sodium ethoxide is added into reaction system, the reaction was continued,
Reaction carries out about 3.5 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product hexichol
Base diethoxy silane, yield 89.65%.
Embodiment 34: the preparation of diphenyl diethoxy silane
Petroleum ether is added in three-neck flask as solvent, 1mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 1.5mol ethyl alcohol and 0.4mol sodium ethoxide are added in flask under inert atmosphere, anti-at 40 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 60%, then 0.3mol sodium ethoxide is added into reaction system, the reaction was continued,
Reaction carries out about 3 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product diphenyl
Diethoxy silane, yield 87.75%.
Embodiment 35: the preparation of diphenyl diethoxy silane
Petroleum ether is added in three-neck flask as solvent, 1mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 1.6mol ethyl alcohol and 0.1mol sodium ethoxide are added in flask under inert atmosphere, anti-at 40 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 40%, then 0.5mol sodium ethoxide is added into reaction system, the reaction was continued,
Reaction carries out about 4 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product diphenyl
Diethoxy silane, yield 85.64%.
Embodiment 36: the preparation of diphenyl diethoxy silane
Petroleum ether is added in three-neck flask as solvent, 1mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 1.6mol ethyl alcohol and 0.4mol sodium ethoxide are added in flask under inert atmosphere, anti-at 40 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 40%, then 0.2mol sodium ethoxide is added into reaction system, the reaction was continued,
Reaction carries out about 4 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product diphenyl
Diethoxy silane, yield 83.9%.
Embodiment 37: the preparation of diphenyl diethoxy silane
Hexamethylene is added in a kettle as solvent, 7.6kg diphenyl dichlorosilane is first added, is uniformly mixed, close
It closes under inert atmosphere, 2kg ethyl alcohol and 0.7kg sodium ethoxide is added in flask, reacted at 40 DEG C, carried out 2 hours in reaction
Afterwards, then into reaction system 0.8kg sodium ethoxide is added, the reaction was continued, and reaction carries out 4 hours altogether.After completion of the reaction, it collects anti-
Product is answered, is filtered, air-distillation, alcoholysis product diphenyl diethoxy silane, yield 89.8% are obtained.
Comparative example 8: the preparation of diphenyl diethoxy silane
In addition to 3.1mol ethyl alcohol is added, it is added without other than sodium ethoxide, is prepared similarly to Example 29, obtain whole production
Object, yield 76.92%.
Comparative example 9: the preparation of diphenyl diethoxy silane
In addition to being prepared other than reaction is initially added into whole ethyl alcohol and sodium ethoxide similarly to Example 29, end is obtained
Product, yield 82.11%.
Embodiment 38: the preparation of diphenyl dipropoxy silane
Petroleum ether is added in three-neck flask as solvent, 1mol diphenyl dichlorosilane is first added, is uniformly mixed, logical
Entering nitrogen to keep environment is that 1.5mol propyl alcohol and 0.3mol sodium propoxide are added in flask under inert atmosphere, anti-at 40 DEG C
It answers, after GC monitors diphenyl dichlorosilane consumption about 40%, then 0.3mol sodium propoxide is added into reaction system, the reaction was continued,
Reaction carries out about 3.5 hours altogether.After completion of the reaction, collecting reaction product, filtering, air-distillation obtain alcoholysis product hexichol
Base dipropoxy silane, yield 76.3%.
Comparative example 10: the preparation of diphenyl dipropoxy silane
In addition to equally being prepared with embodiment 38, obtaining end other than reaction is initially added into whole propyl alcohol and sodium propoxide
Product, yield 78.4%.
As can be seen from the above embodiments, by means of the present invention, the yield of phenyl alkoxysilane reaches
90% or more, this is apparently higher than the prior art, and this method reaction condition is mild, easy to operate, easily controllable, therefore is suitable for
Industrialized production.
Claims (7)
1. a kind of synthetic method of diphenyl diethoxy silane, it is characterised in that be first dissolved in diphenyl dichlorosilane organic
In solvent, ethyl alcohol-alcohol sodium solution is added, is reacted in an inert atmosphere, after reaction carries out a part, ethyl alcohol is added again
Sodium solution, the reaction was continued, and after the completion of reaction, distillation obtains diphenyl diethoxy silane.
2. synthetic method as described in claim 1, which is characterized in that the ethyl alcohol-sodium ethoxide total mole number is by phenylchloride
Silane needs the quantity of chlorine substituent to determine, the alcohol -ol sodium of the corresponding 0.8~1.5mol of each chlorine substituent, preferably 1~
The alcohol -ol sodium of 1.5mol, the alcohol -ol sodium of more preferably 1~1.1mol.
3. synthetic method as described in claim 1, which is characterized in that the molar ratio of alcohol and sodium alkoxide total amount is (1.5~2.5):
1, preferably (1.8~2.2): 1, more preferably 2.1:1.
4. synthetic method as described in claim 1, which is characterized in that the alkoxide amount being added again be alkoxide total amount 40%~
60%, it is added after phenyl chlorosilane consumption 30%~40%.
5. synthetic method as described in claim 1, which is characterized in that its reaction temperature is 10~80 DEG C, when preferably reacting
Between be 4~8 hours.
6. synthetic method as described in claim 1, which is characterized in that organic solvent used in reaction is n-hexane, petroleum
One or both of ether, toluene, dimethylbenzene；The quality of the organic solvent be reaction system gross mass 20%~
60%, more preferable 30%~40%.
7. synthetic method as described in claim 1, which is characterized in that need to be passed through inert gas in reaction to maintain inertia atmosphere
It encloses, which is preferably nitrogen.
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