CN110343129A - The inexpensive method for continuously preparing methyl triacetoxysilane - Google Patents
The inexpensive method for continuously preparing methyl triacetoxysilane Download PDFInfo
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- CN110343129A CN110343129A CN201810281488.8A CN201810281488A CN110343129A CN 110343129 A CN110343129 A CN 110343129A CN 201810281488 A CN201810281488 A CN 201810281488A CN 110343129 A CN110343129 A CN 110343129A
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- Prior art keywords
- nickel
- reactor
- chromium
- acetic acid
- glacial acetic
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- 238000000034 method Methods 0.000 title claims abstract description 34
- TVJPBVNWVPUZBM-UHFFFAOYSA-N [diacetyloxy(methyl)silyl] acetate Chemical compound CC(=O)O[Si](C)(OC(C)=O)OC(C)=O TVJPBVNWVPUZBM-UHFFFAOYSA-N 0.000 title claims abstract description 27
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 76
- 229960000583 acetic acid Drugs 0.000 claims abstract description 33
- 239000003054 catalyst Substances 0.000 claims abstract description 22
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 230000009466 transformation Effects 0.000 claims abstract description 13
- UWGIJJRGSGDBFJ-UHFFFAOYSA-N dichloromethylsilane Chemical compound [SiH3]C(Cl)Cl UWGIJJRGSGDBFJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006356 dehydrogenation reaction Methods 0.000 claims abstract description 8
- 238000000605 extraction Methods 0.000 claims abstract description 5
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 43
- 239000007788 liquid Substances 0.000 claims description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 16
- 235000011054 acetic acid Nutrition 0.000 claims description 14
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 12
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 10
- 229940078494 nickel acetate Drugs 0.000 claims description 10
- 229910000077 silane Inorganic materials 0.000 claims description 9
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims description 8
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 7
- 229910052804 chromium Inorganic materials 0.000 claims description 7
- 239000011651 chromium Substances 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 238000006467 substitution reaction Methods 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical group C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 5
- MCDLETWIOVSGJT-UHFFFAOYSA-N acetic acid;iron Chemical compound [Fe].CC(O)=O.CC(O)=O MCDLETWIOVSGJT-UHFFFAOYSA-N 0.000 claims description 5
- -1 iron ion Chemical class 0.000 claims description 5
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 5
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims description 5
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- WYYQVWLEPYFFLP-UHFFFAOYSA-K chromium(3+);triacetate Chemical compound [Cr+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WYYQVWLEPYFFLP-UHFFFAOYSA-K 0.000 claims description 4
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 4
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims description 4
- 239000005055 methyl trichlorosilane Chemical group 0.000 claims description 4
- GNMQOUGYKPVJRR-UHFFFAOYSA-N nickel(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ni+3].[Ni+3] GNMQOUGYKPVJRR-UHFFFAOYSA-N 0.000 claims description 4
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- DOEHJNBEOVLHGL-UHFFFAOYSA-N trichloro(propyl)silane Chemical group CCC[Si](Cl)(Cl)Cl DOEHJNBEOVLHGL-UHFFFAOYSA-N 0.000 claims description 4
- IVOBGWLJLIDOKO-UHFFFAOYSA-N 2,3-dihydroxybutanedioic acid;nickel Chemical compound [Ni].OC(=O)C(O)C(O)C(O)=O IVOBGWLJLIDOKO-UHFFFAOYSA-N 0.000 claims description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- XEHUIDSUOAGHBW-UHFFFAOYSA-N chromium;pentane-2,4-dione Chemical compound [Cr].CC(=O)CC(C)=O.CC(=O)CC(C)=O.CC(=O)CC(C)=O XEHUIDSUOAGHBW-UHFFFAOYSA-N 0.000 claims description 3
- 125000003963 dichloro group Chemical group Cl* 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- BMGNSKKZFQMGDH-FDGPNNRMSA-L nickel(2+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ni+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O BMGNSKKZFQMGDH-FDGPNNRMSA-L 0.000 claims description 3
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims description 3
- BHIJGQUZXXURRH-ODZAUARKSA-N (z)-but-2-enedioic acid;nickel Chemical compound [Ni].OC(=O)\C=C/C(O)=O BHIJGQUZXXURRH-ODZAUARKSA-N 0.000 claims description 2
- VAIVGJYVKZVQAA-UHFFFAOYSA-N 2-hydroxypropane-1,2,3-tricarboxylic acid;nickel Chemical compound [Ni].OC(=O)CC(O)(C(O)=O)CC(O)=O VAIVGJYVKZVQAA-UHFFFAOYSA-N 0.000 claims description 2
- YFOCIEQUCNIEIA-UHFFFAOYSA-N 2-hydroxypropanoic acid;nickel Chemical compound [Ni].CC(O)C(O)=O YFOCIEQUCNIEIA-UHFFFAOYSA-N 0.000 claims description 2
- OSDWBNJEKMUWAV-UHFFFAOYSA-N Allyl chloride Chemical compound ClCC=C OSDWBNJEKMUWAV-UHFFFAOYSA-N 0.000 claims description 2
- 229910021555 Chromium Chloride Inorganic materials 0.000 claims description 2
- 229910021543 Nickel dioxide Inorganic materials 0.000 claims description 2
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 2
- GFRIWZIMWFPKOB-UHFFFAOYSA-N butanoic acid;nickel Chemical compound [Ni].CCCC(O)=O GFRIWZIMWFPKOB-UHFFFAOYSA-N 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- 238000005660 chlorination reaction Methods 0.000 claims description 2
- 229940090961 chromium dioxide Drugs 0.000 claims description 2
- 229910001430 chromium ion Inorganic materials 0.000 claims description 2
- 229940117975 chromium trioxide Drugs 0.000 claims description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N chromium trioxide Inorganic materials O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 2
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 claims description 2
- XHFVDZNDZCNTLT-UHFFFAOYSA-H chromium(3+);tricarbonate Chemical compound [Cr+3].[Cr+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O XHFVDZNDZCNTLT-UHFFFAOYSA-H 0.000 claims description 2
- IAQWMWUKBQPOIY-UHFFFAOYSA-N chromium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Cr+4] IAQWMWUKBQPOIY-UHFFFAOYSA-N 0.000 claims description 2
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 claims description 2
- AYTAKQFHWFYBMA-UHFFFAOYSA-N chromium(IV) oxide Inorganic materials O=[Cr]=O AYTAKQFHWFYBMA-UHFFFAOYSA-N 0.000 claims description 2
- VQWFNAGFNGABOH-UHFFFAOYSA-K chromium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Cr+3] VQWFNAGFNGABOH-UHFFFAOYSA-K 0.000 claims description 2
- MJFCDPLEATUOPF-UHFFFAOYSA-L dichloronickel;triphenylphosphane Chemical class Cl[Ni]Cl.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 MJFCDPLEATUOPF-UHFFFAOYSA-L 0.000 claims description 2
- IPIIBUIHSKHZTD-UHFFFAOYSA-L diphenylphosphane;ethane;nickel(2+);dichloride Chemical class [Cl-].[Cl-].[Ni+2].CC.C=1C=CC=CC=1PC1=CC=CC=C1.C=1C=CC=CC=1PC1=CC=CC=C1 IPIIBUIHSKHZTD-UHFFFAOYSA-L 0.000 claims description 2
- 229940056319 ferrosoferric oxide Drugs 0.000 claims description 2
- 238000009434 installation Methods 0.000 claims description 2
- 235000014413 iron hydroxide Nutrition 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 claims description 2
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 claims description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 150000002815 nickel Chemical class 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- MRHPUNCYMXRSMA-UHFFFAOYSA-N nickel(2+) oxygen(2-) Chemical compound [O--].[O--].[Ni++] MRHPUNCYMXRSMA-UHFFFAOYSA-N 0.000 claims description 2
- IPLJNQFXJUCRNH-UHFFFAOYSA-L nickel(2+);dibromide Chemical compound [Ni+2].[Br-].[Br-] IPLJNQFXJUCRNH-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- DBJLJFTWODWSOF-UHFFFAOYSA-L nickel(ii) fluoride Chemical compound F[Ni]F DBJLJFTWODWSOF-UHFFFAOYSA-L 0.000 claims description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 2
- NAVSKFYJNZQECG-UHFFFAOYSA-N nickel;propanoic acid Chemical compound [Ni].CCC(O)=O NAVSKFYJNZQECG-UHFFFAOYSA-N 0.000 claims description 2
- QCYXGORGJYUYMT-UHFFFAOYSA-N nickel;triphenylphosphane Chemical compound [Ni].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 QCYXGORGJYUYMT-UHFFFAOYSA-N 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- 150000003751 zinc Chemical class 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000004246 zinc acetate Substances 0.000 claims description 2
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 claims description 2
- 229910021511 zinc hydroxide Inorganic materials 0.000 claims description 2
- 229940007718 zinc hydroxide Drugs 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims 1
- 239000001630 malic acid Substances 0.000 claims 1
- 235000011090 malic acid Nutrition 0.000 claims 1
- HZPNKQREYVVATQ-UHFFFAOYSA-L nickel(2+);diformate Chemical compound [Ni+2].[O-]C=O.[O-]C=O HZPNKQREYVVATQ-UHFFFAOYSA-L 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- 239000006227 byproduct Substances 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- 239000007789 gas Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- VGCXGMAHQTYDJK-UHFFFAOYSA-N Chloroacetyl chloride Chemical compound ClCC(Cl)=O VGCXGMAHQTYDJK-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000003431 cross linking reagent Substances 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 239000000565 sealant Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000013066 combination product Substances 0.000 description 2
- 229940127555 combination product Drugs 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229920002379 silicone rubber Polymers 0.000 description 2
- 239000004945 silicone rubber Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 2
- 239000005052 trichlorosilane Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 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
- 239000004677 Nylon Substances 0.000 description 1
- 150000004075 acetic anhydrides Chemical class 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000919 ceramic Substances 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
- 238000010276 construction Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- RILTWTZTURZUEO-UHFFFAOYSA-N formic acid;nickel Chemical compound [Ni].OC=O RILTWTZTURZUEO-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 210000003296 saliva Anatomy 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000004590 silicone sealant Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 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
- C07F7/1896—Compounds having one or more Si-O-acyl linkages
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The present invention is originally related to a kind of method that low cost continuously prepares methyl triacetoxysilane, belongs to fine chemistry industry and new material technology field；Its step includes: a) catalyst being added in glacial acetic acid and mixes, later mixes dichloromethylsilane with 1 ﹕ 3-7 molar ratio on-line metering with glacial acetic acid；B) reactor group that the reactor for making mixed liquor at the uniform velocity flow through two or two or more is constituted, the system temperature confessed one's crime to each conversion zone of tail is integrally in increment mode, within the scope of 35-115 DEG C, described reactor is made temperature according to the patent application of CN201710956659.8；C) by mixed liquor, further dehydrogenation converts 10-150min in transformation pot, and temperature is 85-135 DEG C；D) by mixed liquor through unreacted glacial acetic acid of negative pressure extraction etc. to get methyl triacetoxysilane.The present invention solves main reaction and dehydrogenation reaction is the double technique problem of invertibity reaction.
Description
Technical field
The present invention relates to the preparation methods of methyl triacetoxysilane, belong to fine chemistry industry and new material technology field.
Background technique
Methyl triacetoxysilane is organosilicon cross-linking agent, is mainly used as the crosslinking of de- acetic acid type organosilicon sealant
The crosslinking agent of agent and single-component room-temperature vulcanized silicone rubber.De- acetic acid type organosilicon sealant is that domestic dosage is maximum organic
One of silicone sealant, since the group of methyl triacetoxysilane is more active compared with other groups such as methoxyl group, ethyoxyl,
De- solution speed is fast, keeps the organosilicon sealant more preferable to adhesive effects such as enhancing aluminium alloy, nylon, glass and ceramics.And methyl
Triacetoxysilane be used as silicone rubber crosslinking agent when, be not required to heating can curing molding, it is with the obvious advantage, be unable to undergo height to some
The component of temperature is also extremely applicable in.
In methyl triacetoxysilane production, since traditional aceticanhydride (acetic anhydride) method production has a large amount of chloroacetic chloride
By-product (it is very big to account for cost ratio), and chloroacetic chloride can inexpensively be obtained from other production in recent years, and the more difficult storehouse of chloroacetic chloride
It deposits, acetic anhydride method production is caused to be obstructed.In addition, though the product total quality of traditional acetic anhydride method production is preferable, chloride ion content is higher,
It influences to use and export in a way.The representative Chinese patent of acetic anhydride method has CN101921289B etc..
In view of this, people transfer study Acetic prepare methyl triacetoxysilane, the method is all with methyl trichlorine at present
Silane is reacted with glacial acetic acid prepares target product, and main stream approach includes solvent acetic acid method and acetic acid vapor method.Though solvent acetic acid method
There is certain isolation HCl gas effect, but still be not enough to effectively prevent the generation (Acetic is invertibity reaction) of back reaction, causes
Reaction time, long by-product was more；Patent CN101323625B is the more typical representative of solvent method, although embodiment (laboratory
Scale) statement product in methyl triacetoxysilane effective content >=94%, but at present producer make similar pilot scale and reality
When production, the effective content of methyl triacetoxysilane is difficult breakthrough 90% in product, some hover always 86%-88% it
Between；It causes by-product impurity to increase because solvent or also being reacted with chlorosilane etc. in addition to the factors such as the reaction time is long；And solvent
The scale of construction and recycling etc., enable consumption is high, low efficiency, in addition there is likely to be pollution of the solvent to environment.Acetic acid vapor method
Advantage is not have to addition solvent, the disadvantage is that the decomposition of material caused by high temperature increases with side reaction, there is also reaction controllings to require height
The situations such as (operation difficulty is big), energy consumption are larger, one way yield is low.
Certainly, Acetic reduces the amount valence of one of primary raw material due to no chloroacetic chloride by-product, still have compared to acetic anhydride method compared with
Big cost advantage；And technically there are also optimization leeway, the method for the patent application including some not yet authorizations with set
It is standby, for example use the reactor of CN201710956659.8 patent application for main equipment etc..But nonetheless, methyl trichlorine at present
The price of silane raises up can still influence the cost of product to a certain extent, and the molecular weight of methyl trichlorosilane relatively large is applied
Measure larger, and 1 moles trichlorosilane can generate 3 moles of HCl gas in reacting, and also digest band to subsequent processing and by-product
Carry out certain pressure.
Summary of the invention
The technical problem to be solved in the present invention is the Improvement requirement and high expensive of the formula for the prior art and technique
The problems such as.
Present invention solves the technical problem that used technical solution, it is to provide a kind of low cost and continuously prepares three second of methyl
The method of acyloxy silane, step include:
A) catalyst is added in liquid glacial acetic acid and is mixed；Dichloromethylsilane is rubbed with liquid glacial acetic acid with 1 ﹕ 3-7 later
You mix than on-line metering；Described catalyst, which is selected from, contains group VIB, the VIIIth race, the Ith B race, II B-group, the VIIth B race mistake
The catalyst for crossing metallic element selects chromium-based catalysts, nickel catalyst, Fe-series catalyst, the catalysis of zinc system from cost performance consideration
One or more of agent, including chromic salts, chromium hydroxide, chromous oxide, chromium dioxide, chrome green, chromium trioxide, contain
Chromium ion complex, nickel salt, nickel hydroxide, nickel monoxide, nickel dioxide, nickel sesquioxide, nickeliferous ionic complex, molysite,
Ferrous hydroxide, iron oxide, ferrous oxide, ferrous oxide, di-iron trioxide, ferroso-ferric oxide, is matched containing iron ion at iron hydroxide
Close object, zinc salt, zinc hydroxide, zinc oxide, object containing zinc ion coordination one or more of, dosage be allyl chloride
The 0.01wt%-0.33wt% of alkane；
B) mixed liquor for mixing step a) on-line metering at the uniform velocity flows through the reactor that two or two or more reactors are constituted
Group, an independent reactor are that entirety or segmentally heating, wherein first reactor upper section or the system temperature of entirety are 35-70
DEG C, the system temperature of last reactor lower section or entirety is 95-115 DEG C, intermediate reactor or reactor region therebetween
System temperature is between described head and the tail temperature；Condenser is connect on each reactor；Described reactor according to
The patent application of CN201710956659.8 is made；
C) by the resulting mixed liquor of step b), further dehydrogenation converts 10-150min, the system temperature of transformation pot in transformation pot
It is 85-135 DEG C；
D) by the resulting mixed liquor of step c) reactor facility or biography made of by CN201710956659.8 patent application
The distillation evaporation installation of system, the unreacted glacial acetic acid of negative pressure extraction and a small amount of other low-boiling-point substances are to get methyl triacetoxyl group
Silane, the glacial acetic acid of recycling are used as subsequent to prepare raw material.
Dichloromethylsilane or methyl hydrogen dichlorosilane, molecular formula CH3SiHCl2；Below by acetic anhydride method, Acetic and
The main reaction equation of the method for the present invention is listed one by one (compare):
CH3SiCl3+3(CH3CO)2O→CH3Si(OCOCH3)3+3C2H3ClO
CH3SiCl3+3CH3COOH→CH3Si(OCOCH3)3+3HCl
CH3SiHCl2+3CH3COOH→CH3Si(OCOCH3)3+2HCl+H2
Not only molecular weight is small (dosage is opposite just few) for dichloromethylsilane, and 1 moles trichlorosilane only generates 2 and rubs in reaction
Your HCl gas；And the producer price of dichloromethylsilane is almost 0 always, compares the methyl trichlorine silicon of one ton of thousands of members
Alkane, cost advantage are obvious.
Preferably, the reactor group that described step b) selects two or more reactors to constitute, and set mixed liquor and flow through
The accumulative total kilometres of the liquid stream hang plate of reactor group are 45-100m, even with the dehydrogenation transformation time of opposite reduction step c)
Step c) is omitted, enables continuous preparation more smooth.
Preferably, described catalyst is the salt and/or its ionic complex of nickel, chromium, iron, including nickel acetate, formic acid
Nickel, nickelous carbonate, nickel chloride, nickelous bromide, nickel fluoride, nickel nitrate, nickel sulfate, lactic acid nickel, propionic acid nickel, butyric acid nickel, citric acid nickel, apple
Tartaric acid nickel, tartaric acid nickel, maleic acid nickel, two (triphenylphosphine) Nickel Chlorides, the bis- diphenylphosphine ethane Nickel Chlorides of 1,2-, four
(triphenylphosphine) nickel, nickel acetylacetonate, chromium acetate, chromium carbonate, chromium chloride, chromium acetylacetonate, ferrous acetate, ferric acetate, chlorination
Iron, ferric acetyl acetonade one or more of；And zinc acetate alternatively property cocatalyst, or part substitute above-mentioned chromium,
The amount of nickel, Fe-series catalyst.
It is furthermore preferred that described catalyst is nickel acetate, nickelous carbonate, nickel chloride, nickel acetylacetonate, chromium acetate, levulinic
Ketone chromium, ferrous acetate, ferric acetate, ferric acetyl acetonade one or more of；Particularly preferred, described catalyst is second
Sour nickel, ferrous acetate, ferric acetyl acetonade one or more of.
Nickel acetate is soluble in acetic acid, is not necessarily to other solvent, and catalytic action is excellent, and comparing nickel chloride will not volume in the product
Outer increase chloride ion, therefore using nickel acetate as first choice.And nickelous carbonate reacts in glacial acetic acid and generates nickel acetate and carbon dioxide gas
Body, and compare nickel hydroxide and will not additionally increase moisture content in system.Ferrous acetate color is shallowly inexpensive.
Preferably, mixed liquor flows through the flow velocity of reactor group in step b), average with described inside reactor conversion zone
Cross section 1m2It is calculated as 0.3-1.2m3/h。
Preferably, in the unreacted glacial acetic acid of step e) negative pressure extraction and other low-boiling-point substances, system temperature 118-
138 DEG C, vacuum degree is more than or equal to -0.098Mpa.
Preferably, first reactor of described step b) reactor group sets up 3-4 bringing-up sections, the system of each bringing-up section
Temperature is gradually incremented by from top to bottom.
Preferably, it in the glacial acetic acid of step a), also added with acetic anhydride, is held under 25-45 DEG C of system temperature after addition
Continuous 1-24h, stirs therebetween or makees the stirring of intermittence；The additional amount of acetic anhydride is the 400wt%- of contained moisture content amount in glacial acetic acid
560wt%。
Industrial acetic contains certain moisture content, and the purpose that acetic anhydride is added is water removal, to prevent material hydrolysis wave
Expense and by-product increase, and then improve product quality (effective content for improving target product), moreover it is possible to effectively reduce equipment knot
Dirt.Both because the molecular weight of acetic anhydride is 5.667 times of water, and under normal circumstances it is not possible that 100% reaction is at acetic acid, therefore set
Relatively suitable ratio.It is reacted are as follows:
(CH3CO)2O+H20→2CH3COOH
Optionally, in step a), part methyl dichloro hydrogen silane is substituted with propyltrichlorosilan and/or methyl trichlorosilane,
Substitution metering is as unit of molal quantity；Meanwhile the dosage of catalyst is accordingly reduced, i.e., still with dichloromethylsilane therein
0.01wt%-0.35wt% metering.
Because the product of 40.5 DEG C of methyl triacetoxysilane sterling molten point, therefore purity is high needs to be made into combination product sometimes, with
It is easy to use.And combination product is directly prepared into propyltrichlorosilan substitution part methyl dichloro hydrogen silane, when use, just need not be multiple
Match, molten point can be greatly reduced in general 8% or more propyltrichlorosilan substitution rate, and final products performance is suitable, substitution rate
Cost is also not much different when lower.And product molten point cannot be reduced with methyl trichlorosilane substitution part methyl dichloro hydrogen silane,
But accordingly reduce the dosage of catalyst.These can make selection appropriate according to actual needs.
Beneficial effects of the present invention are the cost advantage using the dog-cheap byproduct in upstream as one of primary raw material first
It is fairly obvious, and itself by-product HCl reduces 1/3, eases off the pressure to subsequent processing and by-product digestion；Patent application is used simultaneously
Equipment and gas-liquid shunting technique, escape HCl etc. quickly through the ad hoc channel of gas, and reduce the ascending air of reaction generation to liquid
The impact type of phase contacts, and effectively subtracts the generation for the back reaction that disappeared, solves main reaction and dehydrogenation reaction is what invertibity was reacted
Double technique problem causes the effective content of methyl triacetoxysilane in product that can be apparently higher than solvent acetic acid method etc..And
Preferred embodiment is relatively paid attention to detail, and the improvement continuously prepared and unique seamless dewatering process etc. are related to.
Specific embodiment
The following example is only the spiritual description for embodying creation of the invention, is not intended to limit the scope of the invention,
All all changes made within the scope of claims of the present invention even improve, and all fall in the scope of the present invention.
Embodiment 1
1. capital equipment and its parameter
Reactor made of patent application by CN201710956659.8 is 2 (distillation facility exceptions), individually below with anti-
Device I and reactor II is answered to name, reactor I and II is corresponding one on the other in the form of concatenated to be arranged, reactor group is constituted.
The effecting reaction section (being furnished with the section of liquid stream hang plate) of reactor I is highly set as 7m, and liquid stream stroke is corresponding
3 times of vertical height, i.e. liquid stream stroke overall length are 21 m, and gas phase is through to space shared by channel and liquid stream hang plate and its up and down
The ratio between space shared by region is 1:1.7 between plate；Reactor I divides three Duan Jiare, and the high 2.5m temperature setting of upper section is 40 DEG C, middle section
High 2m temperature setting is 55 DEG C, and the high 2.5m temperature setting of lower section is 64 DEG C；Reactor is titanium with material.Condensation is connect on reactor I
Device, and be connected with HCl/water absorption system and exhaust treatment system etc..
The effecting reaction section (being furnished with the section of liquid stream hang plate) of reactor II is highly set as 7m, and liquid stream stroke is phase
3 times for answering vertical height, i.e. liquid stream stroke overall length are 21 m, and gas phase is through to space shared by channel and liquid stream hang plate and thereon
The ratio between space shared by region is 1:1.7 between lower plate；Reactor II divides two sections of heating, and the high 3m temperature setting of upper section is 78 DEG C, under
The high 4m temperature setting of section is 103 DEG C；Reactor is titanium with material.Connect condenser on reactor II, and with HCl/water absorption system and
Exhaust treatment system etc. is connected.
The lower part discharge port of reactor II is connected with transformation pot, and the system temperature of transformation pot is set as 95-110 DEG C, above connects cold
Condenser, and be connected with HCl/water absorption system and exhaust treatment system etc.；Three transformation pots are set, altogether in favor of continuous production.
2. preparation process and its major parameter
A) 1 part of nickel acetate is added to dissolve in 2100 parts of liquid glacial acetic acids and is mixed；Later by dichloromethylsilane and liquid ice
Acetic acid is pumped into pans or mixer through metering pump with 1 ﹕, 4 molar ratio and is sufficiently mixed；
B) reactor I, II is warming up to setting temperature, leads to dry nitrogen and drive air in device (cooperation vacuumizes), and opens condensed system
System and HCl absorption system；Then, mixed liquor step a) on-line metering mixed at the uniform velocity injects the feed system of reactor I
(flow velocity is with I internal-response section average cross-section 1m of reactor2It is calculated as 0.8m3/ h), by liquid distributor continuously by mixed liquor distribution
To the first plate of each column liquid stream hang plate, liquid is under gravity along every block of hang plate nature saliva stream up to reactor I
Bottom；I discharge port of reactor (or directly opening) is opened after 3-10min, and reaction solution is enabled to enter reactor II；Equally, reaction solution
Every block of hang plate is flowed through to the bottom of reactor II；II discharge port of reactor (or directly opening) is opened after 3-10min minutes, is enabled
Reaction solution enters the first transformation pot.
C) the resulting mixed liquor of step b) is made into transformation pot further dehydrogenation and converts 75min, the system temperature of transformation pot
Degree is 102 DEG C；
D) flow velocity of the resulting mixed liquor of step c) and above-mentioned basic synchronization is flowed through by CN201710956659.8 patent application
Manufactured reactor facility, reactor facility effecting reaction section (being furnished with the section of liquid stream hang plate) are highly set as 5m, liquid stream
Stroke is 2.8 times of corresponding vertical height, and whole section of system temperature is 128 DEG C, and vacuum degree is greater than -0.098Mpa, makes in mixed liquor
Unreacted glacial acetic acid and a small amount of other low-boiling-point substance rapid evaporations, the glacial acetic acid of recycling are used as subsequent to prepare raw material；More than steaming
Liquid filtering gets product (or making some subsequent routinely processing according to client).
Through detecting, effective content >=96.2% of methyl triacetoxysilane in product.
It reacts the HCl generated and hydrochloric acid is absorbed with water, Hydrogen collection utilizes, or presses environmental law by exhaust treatment system again
The processing such as rule.
Embodiment 2
It is catalyzed outside divided by nickel chloride equivalent substitution nickel acetate, remaining is the same as embodiment 1.Finally obtain methyl triacetyl in product
The effective content and embodiment 1 of oxysilane are suitable.
Embodiment 3
On the basis of embodiment 1, step a) separately adds 3 parts of acetic anhydrides in 2100 parts of glacial acetic acids, and in vapor tight tank under stirring
42 DEG C are warming up to, stops heat supply and persistently stirs 2h again；It is subsequent to be operated by embodiment 1, finally obtain methyl triacetyl in product
Effective content >=97.6% of oxysilane.
Claims (9)
1. the inexpensive method for continuously preparing methyl triacetoxysilane, it is characterised in that step includes:
A) catalyst is added in liquid glacial acetic acid and is mixed；Dichloromethylsilane is rubbed with liquid glacial acetic acid with 1 ﹕ 3-7 later
You mix than on-line metering；Described catalyst, which is selected from, contains group VIB, the VIIIth race, the Ith B race, II B-group, the VIIth B race mistake
The catalyst for crossing metallic element selects chromium-based catalysts, nickel catalyst, Fe-series catalyst, the catalysis of zinc system from cost performance consideration
One or more of agent, including chromic salts, chromium hydroxide, chromous oxide, chromium dioxide, chrome green, chromium trioxide, contain
Chromium ion complex, nickel salt, nickel hydroxide, nickel monoxide, nickel dioxide, nickel sesquioxide, nickeliferous ionic complex, molysite,
Ferrous hydroxide, iron oxide, ferrous oxide, ferrous oxide, di-iron trioxide, ferroso-ferric oxide, is matched containing iron ion at iron hydroxide
Close object, zinc salt, zinc hydroxide, zinc oxide, object containing zinc ion coordination one or more of, dosage be allyl chloride
The 0.01wt%-0.33wt% of alkane；
B) mixed liquor for mixing step a) on-line metering at the uniform velocity flows through the reactor that two or two or more reactors are constituted
Group, an independent reactor are that entirety or segmentally heating, wherein first reactor upper section or the system temperature of entirety are 35-70
DEG C, the system temperature of last reactor lower section or entirety is 95-115 DEG C, intermediate reactor or reactor region therebetween
System temperature is between described head and the tail temperature；Condenser is connect on each reactor；Described reactor according to
The patent application of CN201710956659.8 is made；
C) by the resulting mixed liquor of step b), further dehydrogenation converts 10-150min, the system temperature of transformation pot in transformation pot
It is 85-135 DEG C；
D) by the resulting mixed liquor of step c) reactor facility or biography made of by CN201710956659.8 patent application
The distillation evaporation installation of system, the unreacted glacial acetic acid of negative pressure extraction and a small amount of other low-boiling-point substances are to get methyl triacetoxyl group
Silane, the glacial acetic acid of recycling are used as subsequent to prepare raw material.
2. the method that low cost as described in claim 1 continuously prepares methyl triacetoxysilane, which is characterized in that described
The reactor group that step b) selects two or more reactors to constitute, and set the liquid stream hang plate that mixed liquor flows through reactor group
Accumulative total kilometres be 45-100m, step c) is omitted even with the dehydrogenation transformation time of opposite reduction step c), enables continuous preparation
It is more smooth.
3. the method that low cost as claimed in claim 1 or 2 continuously prepares methyl triacetoxysilane, which is characterized in that
Described catalyst is the salt and/or its ionic complex of nickel, chromium, iron, including nickel acetate, nickel formate, nickelous carbonate, chlorination
Nickel, nickelous bromide, nickel fluoride, nickel nitrate, nickel sulfate, lactic acid nickel, propionic acid nickel, butyric acid nickel, citric acid nickel, malic acid nickel, tartaric acid
Nickel, maleic acid nickel, two (triphenylphosphine) Nickel Chlorides, the bis- diphenylphosphine ethane Nickel Chlorides of 1,2-, four (triphenylphosphine) nickel, second
Acyl acetone nickel, chromium acetate, chromium carbonate, chromium chloride, chromium acetylacetonate, ferrous acetate, ferric acetate, iron chloride, ferric acetyl acetonade it
One or more of；And zinc acetate alternatively property cocatalyst, or part substitute above-mentioned chromium, nickel, Fe-series catalyst it
Amount.
4. the method that low cost as described in any one of claims 1-3 continuously prepares methyl triacetoxysilane, feature
It is, described catalyst is nickel acetate, nickelous carbonate, nickel chloride, nickel acetylacetonate, chromium acetate, chromium acetylacetonate, acetic acid Asia
Iron, ferric acetate, ferric acetyl acetonade one or more of；Particularly preferred, described catalyst is nickel acetate, acetic acid Asia
Iron, ferric acetyl acetonade one or more of.
5. the method that low cost according to any one of claims 1-4 continuously prepares methyl triacetoxysilane, feature
It is, mixed liquor flows through the flow velocity of reactor group in step b), with described inside reactor conversion zone average cross-section 1m2
It is calculated as 0.3-1.2m3/h。
6. the method that low cost as described in any one in claim 1-5 continuously prepares methyl triacetoxysilane, feature
It is, in the unreacted glacial acetic acid of step e) negative pressure extraction and other low-boiling-point substances, system temperature is 118-138 DEG C, vacuum
Degree is more than or equal to -0.098Mpa.
7. the method that low cost as claimed in any one of claims 1 to 6 continuously prepares methyl triacetoxysilane, feature
Be, first reactor of described step b) reactor group sets up the bringing-up section of 3-4, the system temperature of each bringing-up section from upper and
Under be gradually incremented by.
8. such as the method that the described in any item low costs of claim 1-7 continuously prepare methyl triacetoxysilane, feature
It is, in the glacial acetic acid of step a), also added with acetic anhydride, continues 1-24h after addition under 25-45 DEG C of system temperature,
Between stir or make the stirring of intermittence；The additional amount of acetic anhydride is the 400wt%-560wt% of contained moisture content amount in glacial acetic acid.
9. such as the method that the described in any item low costs of claim 1-8 continuously prepare methyl triacetoxysilane, feature
It is, in step a), part methyl dichloro hydrogen silane, substitution meter is substituted with propyltrichlorosilan and/or methyl trichlorosilane
Amount is as unit of molal quantity；Meanwhile the dosage of catalyst is accordingly reduced, i.e., still with dichloromethylsilane therein
0.01wt%-0.35wt% metering.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114315890A (en) * | 2022-01-05 | 2022-04-12 | 湖北江瀚新材料股份有限公司 | Preparation method of methacryloxypropyl triacetoxysilane |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926856A (en) * | 2015-05-15 | 2015-09-23 | 湖北环宇化工有限公司 | Falling film continuous preparation method of acyloxysilane |
| CN105131028A (en) * | 2015-09-06 | 2015-12-09 | 浙江衢州硅宝化工有限公司 | Preparation method of methyl triethoxysilane |
-
2018
- 2018-04-02 CN CN201810281488.8A patent/CN110343129A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926856A (en) * | 2015-05-15 | 2015-09-23 | 湖北环宇化工有限公司 | Falling film continuous preparation method of acyloxysilane |
| CN105131028A (en) * | 2015-09-06 | 2015-12-09 | 浙江衢州硅宝化工有限公司 | Preparation method of methyl triethoxysilane |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114315890A (en) * | 2022-01-05 | 2022-04-12 | 湖北江瀚新材料股份有限公司 | Preparation method of methacryloxypropyl triacetoxysilane |
| CN114315890B (en) * | 2022-01-05 | 2023-11-17 | 湖北江瀚新材料股份有限公司 | Preparation method of methacryloxypropyl triacetoxy silane |
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