CN102086214B - 一种γ-氯丙基三乙氧基硅烷的生产方法 - Google Patents
一种γ-氯丙基三乙氧基硅烷的生产方法 Download PDFInfo
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- CN102086214B CN102086214B CN 201010590854 CN201010590854A CN102086214B CN 102086214 B CN102086214 B CN 102086214B CN 201010590854 CN201010590854 CN 201010590854 CN 201010590854 A CN201010590854 A CN 201010590854A CN 102086214 B CN102086214 B CN 102086214B
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- reaction
- chloropropyl
- silane
- temperature
- ethanol
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- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 91
- 238000006243 chemical reaction Methods 0.000 claims abstract description 83
- OOXSLJBUMMHDKW-UHFFFAOYSA-N trichloro(3-chloropropyl)silane Chemical compound ClCCC[Si](Cl)(Cl)Cl OOXSLJBUMMHDKW-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000005886 esterification reaction Methods 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 238000004821 distillation Methods 0.000 claims description 35
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- 230000032050 esterification Effects 0.000 claims description 27
- 239000007789 gas Substances 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 238000006386 neutralization reaction Methods 0.000 claims description 8
- 238000005040 ion trap Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000011084 recovery Methods 0.000 claims description 4
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 8
- 230000035484 reaction time Effects 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 20
- 239000012071 phase Substances 0.000 description 19
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 17
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 17
- 239000007921 spray Substances 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 9
- 238000003786 synthesis reaction Methods 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 7
- 238000010992 reflux Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- -1 γ-chloropropyl Chemical group 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000006136 alcoholysis reaction Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 230000007812 deficiency Effects 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- OWXJKYNZGFSVRC-NSCUHMNNSA-N (e)-1-chloroprop-1-ene Chemical compound C\C=C\Cl OWXJKYNZGFSVRC-NSCUHMNNSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 239000006087 Silane Coupling Agent Substances 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 230000009977 dual effect Effects 0.000 description 3
- 235000013312 flour Nutrition 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000007086 side reaction Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 208000012839 conversion disease Diseases 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000005749 Copper compound Substances 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010023126 Jaundice Diseases 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000007806 chemical reaction intermediate Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- DIZMNGDBDDPYEZ-UHFFFAOYSA-N copper phosphoric acid Chemical compound [Cu].P(O)(O)(O)=O DIZMNGDBDDPYEZ-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000005495 investment casting Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920003225 polyurethane elastomer Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Abstract
Description
序号 | 检测项目 | 实施例1 | 实施例2 | 实施例3 |
1 | 外观 | 无色透明液体 | 无色透明液体 | 无色透明液体 |
2 | 含量(wt%) | 99.56 | 99.62 | 99.72 |
3 | 高沸物(wt%) | 0.095 | 0.088 | 0.061 |
4 | 游离氯(以Cl-计) | 32.5×10-6 | 27×10-6 | 19×10-6 |
5 | 色度(Pt-Co比色计) | 10号 | 5号 | 5号 |
Claims (10)
Priority Applications (1)
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CN 201010590854 CN102086214B (zh) | 2010-12-04 | 2010-12-04 | 一种γ-氯丙基三乙氧基硅烷的生产方法 |
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CN 201010590854 CN102086214B (zh) | 2010-12-04 | 2010-12-04 | 一种γ-氯丙基三乙氧基硅烷的生产方法 |
Publications (2)
Publication Number | Publication Date |
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CN102086214A CN102086214A (zh) | 2011-06-08 |
CN102086214B true CN102086214B (zh) | 2013-07-31 |
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Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102432633B (zh) * | 2011-12-07 | 2014-05-07 | 江西晨光新材料有限公司 | 一种氯丙基三乙氧基硅烷醇解工艺 |
CN103709189A (zh) * | 2013-12-06 | 2014-04-09 | 江西晨光新材料有限公司 | 一种无溶剂法制备硫代羧酸酯硅烷偶联剂工艺 |
CN109021006A (zh) * | 2018-09-08 | 2018-12-18 | 杨秀莲 | 一种无污染制备二苯基二乙氧基硅烷的方法 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4173576A (en) * | 1975-07-23 | 1979-11-06 | Dynamit Nobel Aktiengesellschaft | Process for the esterification of chlorosilanes |
CN101648966A (zh) * | 2009-09-03 | 2010-02-17 | 潍坊中业化学有限公司 | 一种同时提高γ-氯丙基三乙氧基硅烷含量及收率的方法 |
CN201614355U (zh) * | 2009-12-25 | 2010-10-27 | 潍坊中狮化工股份有限公司 | γ-氯丙基三乙氧基硅烷酯化反应装置 |
-
2010
- 2010-12-04 CN CN 201010590854 patent/CN102086214B/zh not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4173576A (en) * | 1975-07-23 | 1979-11-06 | Dynamit Nobel Aktiengesellschaft | Process for the esterification of chlorosilanes |
CN101648966A (zh) * | 2009-09-03 | 2010-02-17 | 潍坊中业化学有限公司 | 一种同时提高γ-氯丙基三乙氧基硅烷含量及收率的方法 |
CN201614355U (zh) * | 2009-12-25 | 2010-10-27 | 潍坊中狮化工股份有限公司 | γ-氯丙基三乙氧基硅烷酯化反应装置 |
Non-Patent Citations (2)
Title |
---|
γ-氯丙基三乙氧基硅烷的合成研制;田瑞亭;《山东化工》;20010831;第30卷(第4期);第3-4, 8页, 尤其是第4页2.4部分和表2 * |
田瑞亭.γ-氯丙基三乙氧基硅烷的合成研制.《山东化工》.2001,第30卷(第4期),第4页. |
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