CN110172072A - The method of chloride is removed in a kind of alkoxy silane - Google Patents
The method of chloride is removed in a kind of alkoxy silane Download PDFInfo
- Publication number
- CN110172072A CN110172072A CN201910560871.1A CN201910560871A CN110172072A CN 110172072 A CN110172072 A CN 110172072A CN 201910560871 A CN201910560871 A CN 201910560871A CN 110172072 A CN110172072 A CN 110172072A
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- CN
- China
- Prior art keywords
- chloride
- alkoxy silane
- dosage
- ammonium
- reaction
- Prior art date
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- Granted
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- -1 alkoxy silane Chemical compound 0.000 title claims abstract description 83
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 58
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 44
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 239000000047 product Substances 0.000 claims abstract description 24
- 239000003093 cationic surfactant Substances 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000460 chlorine Substances 0.000 claims abstract description 17
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 17
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 17
- 239000011734 sodium Substances 0.000 claims abstract description 17
- 239000012043 crude product Substances 0.000 claims abstract description 16
- 229910021381 transition metal chloride Inorganic materials 0.000 claims abstract description 9
- 238000004321 preservation Methods 0.000 claims abstract description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 54
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 34
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 235000019441 ethanol Nutrition 0.000 claims description 14
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical group [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 6
- NHGXDBSUJJNIRV-UHFFFAOYSA-M tetrabutylammonium chloride Chemical compound [Cl-].CCCC[N+](CCCC)(CCCC)CCCC NHGXDBSUJJNIRV-UHFFFAOYSA-M 0.000 claims description 6
- 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 description 5
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 5
- 230000001476 alcoholic effect Effects 0.000 claims description 5
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 5
- 125000003545 alkoxy group Chemical group 0.000 claims description 5
- 150000002191 fatty alcohols Chemical class 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- QDYLMAYUEZBUFO-UHFFFAOYSA-N cetalkonium chloride Chemical compound CCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 QDYLMAYUEZBUFO-UHFFFAOYSA-N 0.000 claims description 4
- 229920001296 polysiloxane Polymers 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000005660 chlorination reaction Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 2
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- KHSLHYAUZSPBIU-UHFFFAOYSA-M benzododecinium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 KHSLHYAUZSPBIU-UHFFFAOYSA-M 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 125000002091 cationic group Chemical group 0.000 claims description 2
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 2
- RJMRIDVWCWSWFR-UHFFFAOYSA-N methyl(tripropoxy)silane Chemical compound CCCO[Si](C)(OCCC)OCCC RJMRIDVWCWSWFR-UHFFFAOYSA-N 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 2
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 claims 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 230000003213 activating effect Effects 0.000 claims 1
- 150000001350 alkyl halides Chemical class 0.000 claims 1
- WGQKYBSKWIADBV-UHFFFAOYSA-O benzylaminium Chemical compound [NH3+]CC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-O 0.000 claims 1
- 125000004432 carbon atom Chemical group C* 0.000 claims 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 claims 1
- 229910052759 nickel Inorganic materials 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 10
- 238000003672 processing method Methods 0.000 abstract description 4
- 238000000746 purification Methods 0.000 abstract description 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- 231100000481 chemical toxicant Toxicity 0.000 abstract 1
- 239000002360 explosive Substances 0.000 abstract 1
- 239000003440 toxic substance Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 22
- 239000005046 Chlorosilane Substances 0.000 description 9
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 9
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 7
- 238000009835 boiling Methods 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 238000006136 alcoholysis reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 238000006298 dechlorination reaction Methods 0.000 description 2
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 description 2
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 2
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- AJXBTRZGLDTSST-UHFFFAOYSA-N amino 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)ON AJXBTRZGLDTSST-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 description 1
- 125000001891 dimethoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000012280 lithium aluminium hydride Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000005055 methyl trichlorosilane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 229940038384 octadecane Drugs 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 description 1
- SUBJHSREKVAVAR-UHFFFAOYSA-N sodium;methanol;methanolate Chemical compound [Na+].OC.[O-]C SUBJHSREKVAVAR-UHFFFAOYSA-N 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 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
-
- 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
- C07F7/20—Purification, separation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The present invention relates to a kind of methods that chloride is removed in alkoxy silane, it the described method comprises the following steps: transition metal chloride being added to after being mixed in alkoxy silane crude product, by the first heating period, carried out for the second heating period at higher temperatures again, cationic surfactant heat preservation back flow reaction is added simultaneously, cool down after completion of the reaction, the low-alcohol solution that rudimentary sodium alkoxide is added neutralizes, and then obtains the alkoxy silane product of low chlorine content by rectifying.By the method for the present invention treated alkoxy silane chlorinity down to 3.2ppm hereinafter, conductivity down to 0.52 μ s/cm hereinafter, form and aspect index in APHA30 hereinafter, and high income, product loss late it is small.Processing method of the invention is simple and convenient, low in cost, and is not related to inflammable and explosive or toxic chemical reagent in treatment process, and security risk is not present, and is a kind of method of the industrialization alkoxy silane purification of worth business promotion.
Description
Technical field
The present invention relates to field of organic silicon, and in particular to a kind of method that chloride is removed in alkoxy silane, especially
The method of chloride is removed in electric industry alkoxy silane.
Background technique
Alkoxy silane is big in electric industry demand, it is desirable that purity is very strict, especially if alkoxyl silicone
When containing chloride in alkane, corrosivity is big, causes to corrode to equipment, pipeline, and chloride ion height is easy to cause product conductivity inclined
It is high, therefore chloride needs to remove in time in alkoxy silane.Current general removal method is neutralizer neutralization, with the way of distillation point
From nonvolatile component, but this method can not remove nonionic chlorine, and obviously occur the rising of product form and aspect index after handling etc., limit
The application in electronics, electric field is made.Methyltrimethoxysilane is produced in domestic industry at present mainly uses sodium methoxide two
Secondary response removal method, the specific steps are as follows:
1, the crude product methyltrimethoxysilane that reaction generates, is neutralized with sodium methoxide, and then distillation obtains methyl trimethoxy oxygen
Base silane sterling, purity are generally higher than 99.5%, and non-hydrolyzable chlorinity is generally higher than 200ppm；
2, methyltrimethoxysilane sterling is added in reaction kettle, and the methanol solution of 1.5% silver nitrate is added, reflux
Heating reaction 1h, and, rectifying obtains methyltrimethoxysilane sterling, at this time chlorinity one in sterling in sodium methoxide is added
As can reach 50ppm or so.
But when industrially using sodium methoxide processing method, there is the shortcomings that decomposing product significantly, methyltrimethoxysilane exists
Tetramethoxy-silicane is generated in the process with sodium methoxide chemical combination, causes yield to reduce, by-product increases；Besides using in sodium methoxide
When with agent, often making that treated, siloxanes form and aspect index is increased.
Published technology contents can illustrate chloride removal in alkoxy silane in existing periodical literature, various countries' patent
Status.
Exist in non-patent literature and uses lithium aluminium hydride, the processing method of dibutyl tin, 50% metallic sodium suspension
(Journal of organometallic chemistry, Vol.265,135-139,1984), wherein 50% metallic sodium suspends
Liquid processing, redistillation method is effective, but dangerous, is industrially difficult to carry out.
Deutsche Bundespatent 1530673 discloses in ammonia hydrocarbyl alkoxy silanes are produced, anti-after chlorocarbon based alkoxylation
It answers in mixture, the sodium alkoxide with γ-chloroalkylalkoxylsilane equivalent in mixture is added.In European patent 0282846A2, to containing
A small amount of chloride alkoxy silane is handled with excessive sodium alkoxide, and in organic solvent, for example is reacted in toluene, is then crossed and is filtered out
Salt.In European patent 0532872B1, alkoxy silane is in autoclave, in the presence of excess quantity neutralizer, using alcohol boiling point with
Under upper adjusting pressure, reacted with alcohol.Salt is removed in separation, slips out excessive alcohol.Neutralizer is NH3, organic amine and sodium alkoxide.Above-mentioned item
Part is not suitable for γ-chloroalkylalkoxylsilane, because of NH3, organic amine and sodium alkoxide can react with chlorocarbon base.There are also use in the prior art
The metal salt or steric hindrance sodium alkoxide of bulky amine make neutralizer, in 80 DEG C of processing 1-2h, remove the acid contaminant in alkoxy silane,
Then it distills, this method is at high cost, is difficult to industrialize.Methyl trialkoxysilane is disclosed in Chinese patent 102372733A
Continuous preparation method, be using methyl trichlorosilane as pigment and fatty alcohol alcoholysis after, obtained by neutralization procedure and rectification step
To product, neutralizer uses sodium methoxide, sodium ethoxide, triethylamine and urea.There are also in the prior art with pure silicon and alcohol compound
The method that reaction prepares chloro-free alkoxy silane, for example triethoxy is prepared using industrial silicon and ethyl alcohol as raw material in CN1935649A
Silane separates triethoxysilane using absorption or distilation, then catalytic disproportionation produces monosilane, later again with absorption or suction
Attached method carries out the purification of monosilane.The patent is to avoid the introducing of halogen, but this method cost mistake in the initial feed stage
Height, yield is low, and per kilogram silicon is only capable of 150-250 grams of triethoxysilane of production, can not be suitable for large-scale industrial production.In
State patent CN102199168A discloses a kind of synthesis of chloropropyl triethoxysilane, makes in patent processing chloride process
With a large amount of alcoholic solvent, and neutralized using a large amount of magnesium powders.Chinese patent 107522731A is dechlorination with alchlor
Agent handles methyl triethoxy using aluminium powder as neutralizer, obtains the very low product of chlorinity.But it uses a large amount of
Aluminium powder.Aluminium powder and magnesium powder belong to extremely incendive substance on chemical industry, and can release a large amount of heat, and there are serious when use
Security risk, thus should avoid as far as possible in Chemical Manufacture using.
In conclusion the existing method of chloride removal has many disadvantages in alkoxy silane.Currently, only German
Equal European countries grasp its technology, and chlorinity in alkoxy silane can be made to reach 20ppm or less.Although China has also been ground
Study carefully, but due to technically there is very big defect, substantially maintenance alkoxy silane chlorinity in 50ppm or so, product quality compared with
Difference, therefore the market share is small.Therefore, a kind of method for being simple and efficient and removing chloride in alkoxy silane, great research and development meaning are developed
Justice and commercial value.
Summary of the invention
In view of the above problems, the purpose of the present invention is to provide the sides that chloride is removed in a kind of alkoxy silane
Method, after treatment, in product chlorinity down to 5ppm hereinafter, preferably down to 3.2ppm hereinafter, more preferably down to 2ppm hereinafter,
And high income, product loss late is small, and treated that alkoxy silane form and aspect are lower, and color reaches APHA30 or lower,
And it handles simple and convenient.Above-mentioned purpose of the invention is addressed by the following technical programs:
The method of chloride is removed in a kind of alkoxy silane, comprising the following steps:
Transition metal chloride is added to after being mixed in alkoxy silane crude product, by the first heating period, then more
It was carried out at a temperature of high for the second heating period, while cationic surfactant heat preservation back flow reaction is added, dropped after completion of the reaction
Temperature, the low-alcohol solution that rudimentary sodium alkoxide is added neutralize, and then obtain the alkoxy silane product of low chlorine content by rectifying.
Low chlorine content refers to that after treatment the content of chloride is down to 5ppm hereinafter, preferably down to 3.2ppm in system
Hereinafter, more preferably down to 2ppm or less.
First heating period is that heating steams recycling methanol, and temperature is 70-90 DEG C, heating time 1-3 hour；With/
Or second heating period is again temperature rising reflux reaction, is warming up to 100-120 DEG C, heating time 2-5 hour；And/or it is described
Cooling is to cool the temperature to 30-50 DEG C.
The alkoxy silane is not particularly limited, as long as obtained by chlorosilane and fatty alcohol by alcoholysis reaction
In scope of the alkoxy silane in the present invention about " alkoxy silane ", industrial typical example has methyl trimethoxy oxygroup silicon
Alkane, methyltriethoxysilane, methyl tripropoxy silane, tetramethoxy-silicane, tetraethoxysilane, ethyl trimethoxy silicon
Alkane, ethyl triethoxysilane etc..Especially in electric industry, it is relatively more and right to use methyltrimethoxysilane
There are more strict requirements in the content of wherein chloride.Therefore need to remove chloride in specific embodiment in the present invention
Alkoxy silane chooses methyltrimethoxysilane, but should not be construed as limiting the scope of protection of the present invention, for other
Alkoxy silane, using it is provided by the invention remove chloride method also can achieve similar effect, therefore also this
In the range of invention.
The transition metal chloride is selected from least one of iron chloride, copper chloride, nickel chloride, cobalt chloride, preferably
Iron chloride.
The dosage of the transition metal chloride is the 0.05-0.5% for needing to remove the alkoxy silane quality of chloride,
Preferably 0.1-0.3%.Transition metal chloride dosage can should realize to optimum degree hair in a suitable range
Purpose obviously, if dosage is very little, can not the chloride effectively in removing system can deepen product if dosage is excessive
Color makes form and aspect index be deteriorated.
The cationic surfactant is quaternary cationics class, such as alkyl ammonium halide, aryl
Ammonium halide, alkylaryl ammonium halide, specific adducible example includes but is not limited to octadecyltrimethylammonium chloride, 16
Alkyl trimethyl ammonium chloride, hexadecyl dimethylbenzyl ammonium, hexadecyl dimethylbenzyl ammonium, chlorination dodecyl two
At least one of dimethyl benzyl ammonium, Dodecyl dimethyl benzyl ammonium bromide, tetrabutylammonium chloride, tetrabutylammonium bromide.
The cationic surfactant that quaternary ammonium salt is added is in order to a small amount of in the product crude product stored with metal tank
Dissolved metal ions are complexed, and reduce the form and aspect index of system.Inventor is it has been unexpectedly found that be added a certain amount of quaternary ammonium
Cationic surfactants, in addition to product form and aspect index can be reduced, moreover it is possible to chloride in promotion reduction system to a certain degree
Content further decreases.Reason may be to be formed by metal complex to live with certain catalyzing chlorosilane hydrolysis/alcoholysis
Property, make the non-complete hydrolysis chlorosilane of weight that hydrolysis or alcoholysis occur, it is easy to convert the chlorine in high-boiling components and non-volatile impurity to
The hydrogen chloride for neutralizing discharge, further reduced the content of chloride in system.
The dosage of the cationic surfactant is the 0.01- for needing to remove the alkoxy silane quality of chloride
0.1%, preferably 0.02-0.05%.Cationic surfactant dosage is very few, and product form and aspect index can not be effectively reduced, and
Also it can not be cooperateed with transition metal chloride and play the effect for removing chloride；Cationic surfactant dosage is excessive, instead
It is unfavorable for the removing of chloride in system.
The lower alcohol is the fatty alcohol that carbon atom number is 1-4, preferably methanol, ethyl alcohol, propyl alcohol and butanol.It is described rudimentary
In the low-alcohol solution of sodium alkoxide, the alcohol of the pure and mild lower alcohol solvent of rudimentary sodium alkoxide be may be the same or different, for realizing this
The purpose of invention does not influence.Rudimentary sodium alkoxide is the alcoholic solution that mass percentage concentration is 20-50%, preferably mass percentage concentration
For the alcoholic solution of 30-40%.The dosage of lower alcohol sodium solution is the 0.5- for needing to remove the alkoxy silane quality of chloride
3%, preferably 1-2%.
The neutralization, which refers to, becomes pH9-11 from acidity for pH value of solution.
It is that alkoxy silane and anhydrous ferric trichloride powder are put into reaction kettle in the preferred technical solution of the present invention
In, it is heated at 70-90 DEG C and steams methanol, then proceed to after being warming up to 100-120 DEG C of reflux 1-3h, cetyl is added
Trimethyl ammonium chloride, heat preservation back flow reaction 1-2h are cooled to 30-50 DEG C after completion of the reaction, add 30-40wt% sodium methoxide
Methanol solution react 0.5-1h, be neutralized to crude product pH be 9-11, be then rectifying to obtain the methyl trimethoxy oxygroup silicon of low chlorine again
Alkane sterling；Wherein the dosage of anhydrous ferric chloride is the 0.1-0.2% of alkoxy silane quality, hexadecyltrimethylammonium chloride
Dosage is the 0.02-0.05% of alkoxy silane quality, and the dosage of sodium methoxide solution is the 0.8- of alkoxy silane quality
1.5%.
The principle of the present invention process is as follows:
Being reacted using anhydrous ferric trichloride with alkoxy silane crude product makes non-hydrolytic chlorine be converted into free chloride, so
The metal ion etc. for promoting solution colour to deepen is removed with cationic surfactant reaction afterwards, recycles the methanol of sodium methoxide molten
Liquid, which is further reacted with crude product, removes water-disintegrable chlorine in crude product.By taking methyltrimethoxysilane as an example, detailed process includes following
Step:
(1) industrially, alkoxy silane is usually such as the methyl trimethoxy with being prepared after chlorosilane and fatty alcohol alcoholysis
Oxysilane is to react to be made with methanol using Trichloromethyl silane, few due to containing in raw material of industry Trichloromethyl silane
High-boiling components are measured, a small amount of high-boiling components cannot react completely at this point in the reaction, so that containing unsubstituted complete chlorine in product；
Unsubstituted (methyl dimethoxy oxygroup chlorosilane, dimethyl methyl oxygroup chlorosilane, trim,ethylchlorosilane completely in ferric trichloride and crude product
Deng) chlorine be complexed, heavy metallic salt boiling point is very high, thus complexing chlorine after it is very stable, in rectifying product, since product is
It distills and regathers, therefore it will not be carried into the product steamed, can only stay in last rectifying still bottom；In addition, three
Iron chloride or good effective catalyst and complexing agent make unsubstituted complete chlorosilane be fully converted to alkoxy silane,
Also play the purpose for removing chloride.
(2) since industrial chlorosilane is all the storage of carbon steel storage tank, add when itself containing a large amount of metal ions, and handling chlorine
Heavy metallic salt is entered, so that solution form and aspect are significantly raised, after addition cationic surfactant is complexed, hence it is evident that make solution color
Phase index reduces.Inventor has also been unexpectedly discovered that after a certain amount of cationic surfactant is added, and can not only reduce color
Phase index, moreover it is possible to a certain extent in promotion system chloride removing, possible reason be cationic surfactant and
The complex compound formed after complexing of metal ion also has the activity of certain catalyzing chlorosilane hydrolysis.
(3) certain density lower alcohol sodium solution, such as the methanol solution of 30-40% sodium methoxide are added, at 30-50 DEG C
Lower sodium methoxide is reacted with the chlorine (predominantly hydrogen chloride) of free state in methyltrimethoxysilane, neutralizes the chlorine dissolved in crude product
Methanol is generated, and keeping solution PH is 9-11.
(4) mixture after the reaction was completed passes through rectifying, obtains the sterling of methyltrimethoxysilane, and residue is high boiling in kettle
Point solvent recovery processing.
(5) processing method of the invention is used, chlorinity can be by whole process methyltrimethoxysilane crude product
500ppm is down to 2ppm hereinafter, conductivity is down to 0.2 μ s/cm, and the yield of product is up to 99% or so, and loss late is 1% hereinafter, color
Damp degree reaches APHA10, and treatment process is simple and convenient.
Detailed description of the invention
Fig. 1 is the flow diagram that alkoxy silane of the present invention removes chloride.
Specific embodiment
It is done below in conjunction with method of the specific embodiment to alkoxy silane of the present invention removal chloride further details of
It explains, the alkoxy silane that embodiment uses is methyltrimethoxysilane crude product, this is because used in electric industry
For methyltrimethoxysilane, there are more strict requirements for the content of chloride.Therefore specific embodiment in the present invention
The middle alkoxy silane for needing to remove chloride chooses methyltrimethoxysilane, but should not be understood as protecting model to the present invention
The limitation enclosed also can achieve similar other alkoxy silanes using the method provided by the invention for removing chloride
Effect, it is also within the scope of the invention.
Embodiment 1
2000kg methyltrimethoxysilane crude product (the chromatography methyltrimethoxysilane content that reaction is obtained
91%, chlorinity 520ppm, APHA50) it puts into reaction kettle, 2kg anhydrous ferric trichloride powder is then added in a kettle,
In the case of stirring, 80 DEG C of heat preservation 2h are heated to, methanol is steamed, are continuously heating to 110 DEG C of reflux 2h, octadecane is added
Base trimethyl ammonium chloride 0.4kg continues heat preservation reflux 1.5h；After completion of the reaction；40 DEG C are cooled to, 20kg30% sodium methoxide is added
Methanol solution be stirred to react 0.5h, surveying pH value of solution is 10；Rectifying obtains sterling after further steaming methanol, obtains finished product
1812kg。
Embodiment 2
In the same manner as shown in Example 1, different to be that the dosage of anhydrous ferric trichloride is changed to 3kg, octadecyl three
Ammonio methacrylate 0.6kg.
Embodiment 3
According to method same as Example 2, difference is that the methanol solution dosage of 30% sodium methoxide is changed to 30kg.
Embodiment 4
According to method same as Example 2, difference is that the methanol solution dosage of 30% sodium methoxide is changed to 10kg.
Embodiment 5
According to method same as Example 2, difference is that octadecyltrimethylammonium chloride dosage is changed to 0.2kg.
Embodiment 6
According to method same as Example 2, difference is that octadecyltrimethylammonium chloride dosage is changed to 0.8kg.
Embodiment 7
According to method same as Example 2, difference is that octadecyltrimethylammonium chloride dosage is changed to 1.2kg.
Embodiment 8
According to method same as Example 2, difference is that the dosage of anhydrous ferric chloride is changed to 10kg.
Embodiment 9
According to method same as Example 2, difference is that the dosage of anhydrous ferric chloride is changed to 50kg.
Embodiment 10
According to method same as Example 2, difference is that cationic surfactant replaces with tetrabutylammonium chloride.
Embodiment 11
According to method same as Example 2, difference is that cationic surfactant replaces with hexadecyl two
Dimethyl benzyl ammonium.
Comparative example 1
According to method same as Example 2, difference is to be added without cationic surfactant.
Comparative example 2
2000kg methyltrimethoxysilane crude product (the chromatography methyltrimethoxysilane content that reaction is obtained
91%, chlorinity 520ppm, APHA50) it puts into reaction kettle, 60 DEG C are warming up to, the methanol solution of 30kg30% sodium methoxide is added
It is stirred to react 0.5h, surveying solution PH is 8；Further rectifying obtains sterling, is detected, obtains finished product 1761kg.
The methyltrimethoxysilane obtained to above embodiments and comparative example is tested, and indices are listed in 1 institute of table
Show:
Table 1
| Sample | Purity/% | Yield/% | Chlorinity/ppm | Aqueous solution conductivity/μ s/cm | Form and aspect index |
| Embodiment 1 | 99.58 | 99.14 | 1.5 | 0.28 | APHA20 |
| Embodiment 2 | 99.74 | 99.42 | 1.0 | 0.20 | APHA10 |
| Embodiment 3 | 99.57 | 98.34 | 1.2 | 0.22 | APHA10 |
| Embodiment 4 | 99.55 | 99.39 | 2.1 | 0.36 | APHA20 |
| Embodiment 5 | 99.49 | 99.45 | 1.8 | 0.26 | APHA30 |
| Embodiment 6 | 99.52 | 99.39 | 1.6 | 0.31 | APHA10 |
| Embodiment 7 | 99.54 | 99.43 | 3.2 | 0.52 | APHA10 |
| Embodiment 8 | 99.43 | 99.32 | 2.5 | 0.44 | APHA20 |
| Embodiment 9 | 99.31 | 99.33 | 1.3 | 0.55 | APHA40 |
| Embodiment 10 | 99.62 | 99.42 | 1.5 | 0.23 | APHA10 |
| Embodiment 11 | 99.51 | 99.38 | 1.7 | 0.25 | APHA20 |
| Comparative example 1 | 99.42 | 98.87 | 4.8 | 0.87 | APHA80 |
| Comparative example 2 | 99.08 | 95.59 | 124 | 1.80 | - |
The test of aqueous solution conductivity is the aqueous solution for configuring gained methyltrimethoxysilane to 2wt%, tests it
Conductivity.
The test method reference standard ASTM D1209-2005 of form and aspect index is carried out.
From can be seen that the method for removing chloride in alkoxy silane provided by the invention in 1 data of table, use is anhydrous
Iron chloride and cationic surfactant compounding, play synergistic effect, so that chloride contains in treated alkoxy silane
Amount is greatly lowered, and can achieve 3.2ppm hereinafter, preferred embodiment can achieve 1ppm；And gained alkoxy silane is water-soluble
Liquid conductivity hereinafter, preferred embodiment can achieve 0.2 μ s/cm, also reflects the removing of chloride in 0.55 μ s/cm from side
It is that comparison is thorough.In addition, passing through the test of form and aspect index, according to removing chloride process provided by the invention to alkoxyl silicone
After alkane is handled, form and aspect index is lower, generally in APHA30 hereinafter, preferred embodiment can achieve APHA10, can satisfy
The demand of practical application.In addition, the method for removing chloride of the invention, for the yield of product up to 99.5% or so, loss late is low,
Treatment process is simple and convenient, and the process cost that chloride is removed in alkoxy silane is low, and effect is good, is that one kind is suitble to extensive work
The dechlorination method that industryization is promoted.
Above content is merely a preferred embodiment of the present invention, and is not intended to limit embodiment of the present invention, and this field is general
Logical technical staff's central scope according to the present invention and spirit can very easily carry out corresponding flexible or modification, therefore
Protection scope of the present invention should be subject to protection scope required by claims.
Claims (10)
1. removing the method for chloride in a kind of alkoxy silane, comprising the following steps:
Transition metal chloride is added to after being mixed in alkoxy silane crude product, by the first heating period, then higher
At a temperature of carried out for the second heating period, while be added cationic surfactant heat preservation back flow reaction, cool down after completion of the reaction, add
The low-alcohol solution for entering rudimentary sodium alkoxide neutralizes, and then obtains the alkoxy silane product of low chlorine content by rectifying.
2. the method as described in claim 1, which is characterized in that first heating period is that heating steams recycling methanol, temperature
Degree is 70-90 DEG C, heating time 1-3 hour；And/or second heating period is again temperature rising reflux reaction, is warming up to 100-
120 DEG C, heating time 2-5 hour；And/or the cooling is to cool the temperature to 30-50 DEG C.
3. the method as described in claim 1, which is characterized in that the alkoxy silane includes methyltrimethoxysilane, first
Ethyl triethoxy silicane alkane, methyl tripropoxy silane, tetramethoxy-silicane, tetraethoxysilane, ethyl trimethoxy silane, second
Ethyl triethoxy silicane alkane.
4. the method as described in claim 1, which is characterized in that the transition metal chloride is selected from iron chloride, copper chloride, chlorine
Change at least one of nickel, cobalt chloride, preferably iron chloride.
5. method as claimed in claim 4, which is characterized in that the dosage of the transition metal chloride is to need to remove chlorination
The 0.05-0.5% of the alkoxy silane quality of object, preferably 0.1-0.3%.
6. the method as described in claim 1, which is characterized in that the cationic surfactant is quaternary ammonium salt cationic table
Face activating agent class.
7. the method for claim 7, which is characterized in that the quaternary cationics class is selected from alkyl halide
Change at least one of ammonium, aryl ammonium halide, alkylaryl ammonium halide, preferably octadecyltrimethylammonium chloride, hexadecane
Base trimethyl ammonium chloride, hexadecyl dimethylbenzyl ammonium, hexadecyl dimethylbenzyl ammonium, chlorination dimethyl
At least one of base benzyl ammonium, Dodecyl dimethyl benzyl ammonium bromide, tetrabutylammonium chloride, tetrabutylammonium bromide.
8. the method for claim 7, which is characterized in that the dosage of the cationic surfactant is to need to go to dechlorinate
The 0.01-0.1% of the alkoxy silane quality of compound, preferably 0.02-0.05%.
9. the method as described in claim 1, which is characterized in that the lower alcohol is the fatty alcohol that carbon atom number is 1-4, preferably
For methanol, ethyl alcohol, propyl alcohol and butanol；And/or the rudimentary sodium alkoxide is the alcoholic solution that mass percentage concentration is 20-50%, preferably
The alcoholic solution for being 30-40% for mass percentage concentration；The dosage of lower alcohol sodium solution is the alkoxyl silicone for needing to remove chloride
The 0.5-3% of alkane quality, preferably 1-2%.
10. a kind of method for removing chloride in alkoxy silane is to put into alkoxy silane and anhydrous ferric trichloride powder
It in reaction kettle, is heated at 70-90 DEG C and steams methanol, then proceed to after being warming up to 100-120 DEG C of reflux 1-3h, be added ten
Six alkyl trimethyl ammonium chlorides, heat preservation back flow reaction 1-2h are cooled to 30-50 DEG C after completion of the reaction, add 30-40wt%
The methanol solution of sodium methoxide reacts 0.5-1h, and being neutralized to crude product pH is 9-11, is then rectifying to obtain the alkoxyl silicone of low chlorine again
Alkane sterling；Wherein the dosage of anhydrous ferric chloride is the 0.1-0.2% of alkoxy silane quality, hexadecyltrimethylammonium chloride
Dosage is the 0.02-0.05% of alkoxy silane quality, and the dosage of sodium methoxide solution is the 0.8- of alkoxy silane quality
1.5%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115490719A (en) * | 2022-11-22 | 2022-12-20 | 江苏南大光电材料股份有限公司 | Purification method of alkoxy silane composition |
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| US4697027A (en) * | 1985-11-14 | 1987-09-29 | Toray Silicon Co., Ltd. | Method for purifying alkoxysilane |
| JPH02237601A (en) * | 1989-03-09 | 1990-09-20 | Tonen Corp | Method for removing chlorine in alkoxysilane |
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| CN115490719A (en) * | 2022-11-22 | 2022-12-20 | 江苏南大光电材料股份有限公司 | Purification method of alkoxy silane composition |
| WO2024109453A1 (en) * | 2022-11-22 | 2024-05-30 | 江苏南大光电材料股份有限公司 | Purification method for alkoxy silane composition |
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