PL405584A1 - Siloxane-silsesquioxane resins and method for obtaining them - Google Patents
Siloxane-silsesquioxane resins and method for obtaining themInfo
- Publication number
- PL405584A1 PL405584A1 PL40558413A PL40558413A PL405584A1 PL 405584 A1 PL405584 A1 PL 405584A1 PL 40558413 A PL40558413 A PL 40558413A PL 40558413 A PL40558413 A PL 40558413A PL 405584 A1 PL405584 A1 PL 405584A1
- Authority
- PL
- Poland
- Prior art keywords
- reaction
- siloxane
- stage
- silsesquioxane resins
- addition
- Prior art date
Links
- 238000000034 method Methods 0.000 title abstract 5
- 239000011347 resin Substances 0.000 title abstract 5
- 229920005989 resin Polymers 0.000 title abstract 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract 3
- 238000006243 chemical reaction Methods 0.000 abstract 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 abstract 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract 2
- 150000001336 alkenes Chemical class 0.000 abstract 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 abstract 2
- -1 glycidoxypropyl Chemical group 0.000 abstract 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 abstract 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract 2
- 229910052697 platinum Inorganic materials 0.000 abstract 2
- 238000003756 stirring Methods 0.000 abstract 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 abstract 2
- 239000004593 Epoxy Substances 0.000 abstract 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 abstract 1
- 125000000217 alkyl group Chemical group 0.000 abstract 1
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 abstract 1
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 abstract 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 abstract 1
- 125000000524 functional group Chemical group 0.000 abstract 1
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 238000006459 hydrosilylation reaction Methods 0.000 abstract 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 abstract 1
- 239000012044 organic layer Substances 0.000 abstract 1
- 238000005191 phase separation Methods 0.000 abstract 1
- 239000003495 polar organic solvent Substances 0.000 abstract 1
- 150000003283 rhodium Chemical class 0.000 abstract 1
- 229910052703 rhodium Inorganic materials 0.000 abstract 1
- 239000010948 rhodium Substances 0.000 abstract 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
Landscapes
- Silicon Polymers (AREA)
Abstract
Przedmiotem wynalazku są żywice siloksanowo-silseskwioksanowe zawierające organiczne grupy funkcyjne o ogólnej strukturze przedstawionej na schemacie 1, na którym R oznacza grupę metylową, etylową, lub fenylową, R1 oznacza organiczną grupę funkcyjną alkilową, oktafluoropentyloksypropylową, glicydoksypropylową, metakryloksypropylową, epoksycykloheksylową, chloropropylową lub hydroksypropylową, a n przyjmuje wartości w zakresie od 0 do 8, oraz sposób ich otrzymywania. Sposób polega na tym, że prowadzi się dwuetapowy proces, w którym najpierw wodno-metanolowy lub wodno-etanolowy roztwór oktaanionu o wzorze 2, który otrzymuje na drodze kondensacji hydrolitycznej tetraetoksysilanu w obecności metanolu lub etanolu oraz wody i stechiometrycznej ilości wodorotlenku tetra-metyloamoniowego, wkrapla się do roztworu dichlorosilanu o ogólnym wzorze 3, w którym R oznacza grupę metylową, etylową lub fenylową, w niepolarnym rozpuszczalniku organicznym, korzystnie heksanie, benzenie lub toluenie, o stężeniu stanowiącym 2 do 16 krotny nadmiar molowy w przeliczeniu na mol oktaanionu, przy czym układ reakcyjny utrzymuje się w zakresie temperatur od 10 do 0°C, ponadto reakcję prowadzi się przez 2 do 6 godzin od zakończenia wkraplania substratu silnie mieszając a następnie pozostawia bez mieszania w celu rozdzielenia faz, po czym po separacji faz zbiera się warstwę organiczną, z której znanymi sposobami izoluje się produkt W drugim etapie funkcyjne olefiny poddaje się katalitycznej reakcji hydrosililowania za pomocą otrzymanych w pierwszym etapie żywic siloksanowosilseskwioksanowych, przy czym korzystne jest użycie 50 do 100% nadmiaru molowego olefiny względem żywicy, a jako katalizatory stosuje się kompleksy platyny lub rodu, w ilości od 10-4 do 10-6 mola rodu lub platyny na 1 mol ugrupowań Si-H występujących w żywicy, ponadto reakcję prowadzi się w zakresie temperatur od 25-120°C, do zakończenia procesu, w układzie otwartym, pod ciśnieniem atmosferycznym, jest w celu całkowitego przereagowania wiązań Si-H.The present invention relates to siloxane-silsesquioxane resins containing organic functional groups with the general structure shown in Scheme 1, wherein R is a methyl, ethyl or phenyl group, R 1 is an organic alkyl, octafluoropentyloxypropyl, glycidoxypropyl, methacryloxypropyl, epoxy cyclohexyl, or hydroxyl group an takes values in the range of 0 to 8, and how they are obtained. The method consists in carrying out a two-stage process in which first an aqueous methanol or water-ethanol solution of the octaanion of formula II, which receives by hydrolytic condensation of tetraethoxysilane in the presence of methanol or ethanol and water and a stoichiometric amount of tetra-methylammonium hydroxide, dropwise to a solution of dichlorosilane of general formula 3, wherein R is a methyl, ethyl or phenyl group, in a non-polar organic solvent, preferably hexane, benzene or toluene, at a concentration of 2 to 16 times the molar excess based on the mole of octaanion, the system the reaction is maintained in the temperature range from 10 to 0 ° C, in addition, the reaction is carried out for 2 to 6 hours after completion of the dropwise addition of the substrate with strong stirring and then left without stirring to separate the phases, after which, after phase separation, an organic layer is collected, from which the product is isolated in the second stage by known methods functional olefins are subjected to a catalytic hydrosilylation reaction using siloxane-silsesquioxane resins obtained in the first stage, with a 50 to 100% molar excess of olefin relative to the resin being preferred, and platinum or rhodium complexes in the amount of 10-4 to 10- 6 moles of rhodium or platinum per 1 mole of Si-H moieties present in the resin, in addition, the reaction is carried out in the temperature range from 25-120 ° C, until the process is complete, in an open system at atmospheric pressure, to completely react the Si-H bonds H.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PL405584A PL222441B1 (en) | 2013-10-09 | 2013-10-09 | Siloxane-silsesquioxane resins and method for obtaining them |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PL405584A PL222441B1 (en) | 2013-10-09 | 2013-10-09 | Siloxane-silsesquioxane resins and method for obtaining them |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| PL405584A1 true PL405584A1 (en) | 2015-04-13 |
| PL222441B1 PL222441B1 (en) | 2016-07-29 |
Family
ID=52781967
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PL405584A PL222441B1 (en) | 2013-10-09 | 2013-10-09 | Siloxane-silsesquioxane resins and method for obtaining them |
Country Status (1)
| Country | Link |
|---|---|
| PL (1) | PL222441B1 (en) |
-
2013
- 2013-10-09 PL PL405584A patent/PL222441B1/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| PL222441B1 (en) | 2016-07-29 |
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