CN114149462A - 一种苯基烷氧基硅烷的制备方法 - Google Patents
一种苯基烷氧基硅烷的制备方法 Download PDFInfo
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- -1 phenyl alkoxy silane Chemical compound 0.000 title claims abstract description 37
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 46
- 150000001555 benzenes Chemical class 0.000 claims abstract description 9
- 239000000706 filtrate Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 8
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical class [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 12
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 11
- QARVLSVVCXYDNA-UHFFFAOYSA-N bromobenzene Chemical compound BrC1=CC=CC=C1 QARVLSVVCXYDNA-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
- 150000007530 organic bases Chemical class 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- BDAWXSQJJCIFIK-UHFFFAOYSA-N potassium methoxide Chemical compound [K+].[O-]C BDAWXSQJJCIFIK-UHFFFAOYSA-N 0.000 claims description 3
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 229910052754 neon Inorganic materials 0.000 claims description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract description 4
- 239000012295 chemical reaction liquid Substances 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 125000003545 alkoxy group Chemical group 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- CVQVSVBUMVSJES-UHFFFAOYSA-N dimethoxy-methyl-phenylsilane Chemical compound CO[Si](C)(OC)C1=CC=CC=C1 CVQVSVBUMVSJES-UHFFFAOYSA-N 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 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 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 description 3
- REQXNMOSXYEQLM-UHFFFAOYSA-N methoxy-dimethyl-phenylsilane Chemical compound CO[Si](C)(C)C1=CC=CC=C1 REQXNMOSXYEQLM-UHFFFAOYSA-N 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 229920002050 silicone resin Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- RVBVJEZJXBZDON-UHFFFAOYSA-N trimethoxy-[methoxy(dimethyl)silyl]silane Chemical compound CO[Si](C)(C)[Si](OC)(OC)OC RVBVJEZJXBZDON-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000007818 Grignard reagent Substances 0.000 description 2
- 238000006136 alcoholysis reaction Methods 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000004795 grignard reagents Chemical class 0.000 description 2
- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 description 2
- XJWOWXZSFTXJEX-UHFFFAOYSA-N phenylsilicon Chemical compound [Si]C1=CC=CC=C1 XJWOWXZSFTXJEX-UHFFFAOYSA-N 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 2
- OKAMTPRCXVGTND-UHFFFAOYSA-N 2-methoxyoxolane Chemical compound COC1CCCO1 OKAMTPRCXVGTND-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- GTPDFCLBTFKHNH-UHFFFAOYSA-N chloro(phenyl)silicon Chemical compound Cl[Si]C1=CC=CC=C1 GTPDFCLBTFKHNH-UHFFFAOYSA-N 0.000 description 1
- MVPPADPHJFYWMZ-IDEBNGHGSA-N chlorobenzene Chemical group Cl[13C]1=[13CH][13CH]=[13CH][13CH]=[13CH]1 MVPPADPHJFYWMZ-IDEBNGHGSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- RYQFGLPMGZOIIN-UHFFFAOYSA-N dimethoxy-[(2-methylpropan-2-yl)oxy]silane Chemical compound CO[SiH](OC)OC(C)(C)C RYQFGLPMGZOIIN-UHFFFAOYSA-N 0.000 description 1
- BQLQQEHXQQLKEV-UHFFFAOYSA-N dimethoxy-methyl-trimethylsilylsilane Chemical compound CO[Si](C)(OC)[Si](C)(C)C BQLQQEHXQQLKEV-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- JEWCZPTVOYXPGG-UHFFFAOYSA-N ethenyl-ethoxy-dimethylsilane Chemical compound CCO[Si](C)(C)C=C JEWCZPTVOYXPGG-UHFFFAOYSA-N 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- AKYUXYJGXHZKLL-UHFFFAOYSA-N triethoxy(triethoxysilyl)silane Chemical compound CCO[Si](OCC)(OCC)[Si](OCC)(OCC)OCC AKYUXYJGXHZKLL-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- C07F7/08—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
-
- 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
- C07F7/1876—Preparation; Treatments not provided for in C07F7/20 by reactions involving the formation of Si-C linkages
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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
- C07F7/08—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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
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Abstract
本发明公开了一种苯基烷氧基硅烷的制备方法,通过将烷氧基硅烷及有机强碱加入反应釜中,通入惰性气体保护,搅拌均匀,温度维持在20‑60℃,再同时分别滴加卤代苯及烷氧基取代的二硅烷。滴加2‑4h,继续反应4‑6h。反应后的反应液,先过滤,滤液经过精馏分离苯基烷氧基硅烷及烷氧基硅烷。本发明采用烷氧基硅烷作为溶剂,可以有效溶解有机强碱,同时和卤代苯、烷氧基二硅烷有很好的互溶性,有利于反应的进行。反应条件温和、安全易操作。
Description
技术领域
本发明涉及一种有机硅烷的制备方法,更具体是涉及一种苯基烷氧基硅烷的制备方法。
背景技术
苯基烷氧基硅烷是指硅原子上直接链接苯基和烷氧基两种功能基团的特殊单体。苯基烷氧基硅烷是一种重要的有机硅化合物,是制备苯基硅树脂、苯基硅油、苯基硅橡胶的主要原料之一,它对改善有机硅聚合物的性能,特别是耐热性、耐辐射性、化学稳定性、折射率等的作用十分明显。随着有机硅产业的发展,有机硅应用领域的扩大,苯基硅烷的的需求快速增长。
苯基烷氧基硅烷的制备,主要有格氏试剂法、钠缩合法、和醇解法等方法。其中格氏试剂法生产甲基苯基二甲氧基硅烷,工艺简洁,收率较高,所得的产品质量比较好。但制备条件比较严格。所使用的金属镁要求表面干净,氧化程度要小。钠缩合法制备甲基苯基二甲氧基硅烷反应条件温合,容易控制,整个工艺操作也比较简单,且原料较便宜、易于获得。但反应中使用到金属钠,有一定的危险性,对生产中的贮存和使用都提出更髙的要求。醇解法可一步合成甲基苯基二甲氧基硅烷反应,工艺简单。关键点是如何尽快地将生成的HCl及时地从反应体系中移除,但其本身需要使用苯基氯硅烷,不能实现从甲基单体到苯基单体的转化。
发明内容
为了解决制备苯基烷氧基硅烷制备中原料要求严格且具有危险性的问题,采用烷氧基二硅烷和卤代苯、有机强碱反应制备苯基烷氧基硅烷。反应条件温和,反应物不存在重大储存和使用安全问题。
一种苯基烷氧基硅烷的制备方法,具有如下步骤:(1)将烷氧基硅烷及有机强碱加入反应釜中,通入惰性气体保护,搅拌均匀,温度维持在20-60℃,再同时分别滴加卤代苯及烷氧基取代的二硅烷,滴加2-4h,继续反应4-6h。(2)反应后的反应液,先过滤,滤液经过精馏分离出苯基烷氧基硅烷及烷氧基硅烷。
烷氧基硅烷为硅酸四甲酯、硅酸四乙酯、甲基三甲氧基硅烷、二甲基二乙氧基硅烷、甲基三乙氧基硅烷,二甲基二乙氧基硅烷中的一种或其混合物。
有机强碱为醇钠或醇钾,具体的为甲醇钠、乙醇钠、甲醇钾。
惰性气体为氮气、氦气、氖气或氩气中的一种。
卤代苯为氯苯或溴苯或其混合物。
烷氧基取代的二硅烷、有机强碱与卤代苯的摩尔比为1:1-1.2:1-1.2。
有机烷氧基硅烷与有机强碱的的质量比为3-8:1。
本发明同现有技术相比其优点在于:
1.采用烷氧基硅烷作为溶剂,可以有效溶解有机强碱,同时和卤代苯、烷氧基二硅烷有很好的互溶性,有利于反应的进行。
2.烷氧基硅烷不与反应体系发生反应,没有其它副产物产生。
3.烷氧基二硅烷和卤代苯在有机强碱存在下反应生成苯基烷氧基硅烷及烷氧基硅烷,采用烷氧基硅烷为溶剂,减少了反应结束后反应液中的化合物种类,后续精馏减少了精馏步数。
4.反应结束后产物可以不精馏,直接经水解缩合制备甲基苯基硅树脂。
5.反应条件温和、有机强碱相对于单质钠更安全易操作。
具体实施方式
实施例1
将甲基三甲氧基硅烷400g及甲醇钠1.1mol加入反应釜中,通入氮气保护,搅拌均匀,温度维持在20℃,再同时分别滴加氯苯1.2mol及二甲基四甲氧基二硅烷1mol。滴加2h,继续反应6h。反应后的反应液,先过滤,滤液经过精馏分离出甲基苯基二甲氧基硅烷及甲基三甲氧基硅烷。甲基苯基二甲氧基硅烷收率45.6%,甲基三甲氧基硅烷收率95.7%。
实施例2
将硅酸四乙酯250g及乙醇钠1.2mol加入反应釜中,通入氦气保护,搅拌均匀,温度维持在35℃,再同时分别滴加氯苯1mol及六乙氧基二硅烷1mol。滴加3h,继续反应5h。反应后的反应液,先过滤,滤液经过精馏分离出苯基三乙氧基硅烷及硅酸四乙酯。苯基三乙氧基硅烷收率40.6%,硅酸四乙酯收率93.4%。
实施例3
将二甲基二甲氧基硅烷300g及甲醇钾1mol加入反应釜中,通入氮气保护,搅拌均匀,温度维持在50℃,再同时分别滴加溴苯1.1mol及四甲基二甲氧基二硅烷1mol。滴加4h,继续反应4h。反应后的反应液,先过滤,滤液经过精馏分离出二甲基苯基甲氧基硅烷及二甲基二甲氧基硅烷。二甲基苯基甲氧基硅烷收率60.7%,二甲基二甲氧基硅烷收率98.8%。
实施例4
将甲基三甲氧基硅烷400g及甲醇钠1.1mol加入反应釜中,通入氮气保护,搅拌均匀,温度维持在60℃,再同时分别滴加溴苯1.1mol及三甲基三甲氧基二硅烷1mol。滴加2h,继续反应6h。反应后的反应液,先过滤,滤液经过精馏分离出反应产物及有机溶剂。二甲基苯基甲氧基硅烷收率54.6%,甲基三甲氧基硅烷收率96.7%。
对比例1
将甲苯400g及甲醇钠1.1mol加入反应釜中,通入氮气保护,搅拌均匀,温度维持在20℃,再同时分别滴加氯苯1.2mol及二甲基四甲氧基二硅烷1mol。滴加2h,继续反应6h。反应后的反应液,先过滤,滤液经过精馏分离出甲苯、甲基苯基二甲氧基硅烷及甲基三甲氧基硅烷。甲基苯基二甲氧基硅烷收率4.5%,甲基三甲氧基硅烷收率93.8%。
对比例2
将四氢呋喃400g及甲醇钠1.1mol加入反应釜中,通入氮气保护,搅拌均匀,温度维持在20℃,再同时分别滴加氯苯1.2mol及二甲基四甲氧基二硅烷1mol。滴加2h,继续反应6h。反应后的反应液,先过滤,滤液GC-MS分析生成副产物2-甲氧基四氢呋喃(5.2%)。经过精馏分离出四氢呋喃、甲基苯基二甲氧基硅烷及甲基三甲氧基硅烷。甲基苯基二甲氧基硅烷收率42.6%,甲基三甲氧基硅烷收率95.5%。
实施例5-21
将实施例1-4中反应得到混合物分别和甲基三甲氧基硅烷、二甲基乙烯基乙氧基硅烷加入反应釜中,加入30g含HCl为153μL/L的稀盐酸,搅拌并升温至80反应3h,100℃蒸出乙醇及水,得到甲基苯基硅树脂。采用GB/T 6488-2008规定的方法测试折光率。采用《有机硅树脂及其应用》-赵陈超,化学工业出版社,2011.8(2018.8重印),第47页检测热老化稳定性半衰期/h。
具体物料加入量如表1。
表1.原料配比数据表
测得的折光率及半衰期数据如表2.
表2.折光率数据表
Claims (8)
1.一种苯基烷氧基硅烷的制备方法,其特征在于,具有如下步骤:
(1)将烷氧基硅烷及有机强碱加入反应釜中,通入惰性气体保护,搅拌均匀,温度维持在20-60℃,再同时分别滴加卤代苯及烷氧基取代的二硅烷,滴加2-4h,继续反应4-6h;
(2)反应后的反应液,先过滤,滤液经过精馏分离得到苯基烷氧基硅烷及烷氧基硅烷。
2.根据权利要求1所述的苯基烷氧基硅烷的制备方法,其特征在于步骤(1)中所述的烷氧基硅烷为硅酸四甲酯、硅酸四乙酯、甲基三甲氧基硅烷、二甲基二乙氧基硅烷、甲基三乙氧基硅烷,二甲基二乙氧基硅烷中的一种或其混合物。
3.根据权利要求1所述的苯基烷氧基硅烷的制备方法,其特征在于步骤(1)中所述的有机强碱为醇钠或醇钾,包括甲醇钠、乙醇钠、或甲醇钾。
4.根据权利要求1所述的苯基烷氧基硅烷的制备方法,其特征在于步骤(1)中所述的惰性气体为氮气、氦气、氖气或氩气中的一种。
5.根据权利要求1所述的苯基烷氧基硅烷的制备方法,其特征在于步骤(1)中所述的卤代苯为氯苯或溴苯或其混合物。
6.根据权利要求1所述的苯基烷氧基硅烷的制备方法,其特征在于步骤(1)中所述的烷氧基取代的二硅烷、有机强碱与卤代苯的摩尔比为1:1-1.2:1-1.2。
7.根据权利要求1所述的苯基烷氧基硅烷的制备方法,其特征在于步骤(1)中所述的烷氧基硅烷与有机强碱的质量比为3-8:1。
8.根据权利要求1所述的苯基烷氧基硅烷的制备方法,其特征在于步骤(1)中所述的烷氧基取代的二硅烷分子式为(CH3)n(RO)6-nSi2,R为甲基,4≥n≥0。
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CN107540707A (zh) * | 2017-07-24 | 2018-01-05 | 山东东岳有机硅材料有限公司 | 有机硅单体的制备方法 |
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