NO894361L - DURABLE STORAGE STABLE RTV-1K MASSES. - Google Patents
DURABLE STORAGE STABLE RTV-1K MASSES.Info
- Publication number
- NO894361L NO894361L NO89894361A NO894361A NO894361L NO 894361 L NO894361 L NO 894361L NO 89894361 A NO89894361 A NO 89894361A NO 894361 A NO894361 A NO 894361A NO 894361 L NO894361 L NO 894361L
- Authority
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- Norway
- Prior art keywords
- weight
- masses
- chalk
- masses according
- precipitated
- Prior art date
Links
- 238000003860 storage Methods 0.000 title description 11
- 239000010936 titanium Substances 0.000 claims abstract description 11
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000007717 exclusion Effects 0.000 claims abstract description 9
- 239000000945 filler Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 6
- 229920001971 elastomer Polymers 0.000 claims abstract description 6
- 239000000806 elastomer Substances 0.000 claims abstract description 6
- 150000002148 esters Chemical class 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims abstract description 4
- 239000000049 pigment Substances 0.000 claims abstract description 4
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 10
- -1 ester compounds Chemical class 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 7
- 238000004132 cross linking Methods 0.000 claims description 5
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 229910001385 heavy metal Inorganic materials 0.000 claims description 3
- 230000002209 hydrophobic effect Effects 0.000 claims description 3
- 230000001698 pyrogenic effect Effects 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 150000002736 metal compounds Chemical class 0.000 claims description 2
- 125000005624 silicic acid group Chemical class 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 4
- 239000000565 sealant Substances 0.000 abstract description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 6
- 229920002379 silicone rubber Polymers 0.000 description 6
- 239000013522 chelant Substances 0.000 description 5
- 229920001296 polysiloxane Polymers 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 235000015927 pasta Nutrition 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 150000004756 silanes Chemical class 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 125000003545 alkoxy group Chemical group 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000004971 Cross linker Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- KKSAZXGYGLKVSV-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO KKSAZXGYGLKVSV-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000004922 lacquer Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000005055 methyl trichlorosilane Substances 0.000 description 1
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K3/1006—Materials in mouldable or extrudable form for sealing or packing joints or covers characterised by the chemical nature of one of its constituents
- C09K3/1018—Macromolecular compounds having one or more carbon-to-silicon linkages
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
- C08G77/16—Polysiloxanes containing silicon bound to oxygen-containing groups to hydroxyl groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
- C08G77/18—Polysiloxanes containing silicon bound to oxygen-containing groups to alkoxy or aryloxy groups
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Paints Or Removers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
! Linder utelukkelse av fuktighet lagringsdyktige og ved omgivelsestemperatur under innvirkning av vann eller atmosfærisk luft til strekkfaste elastomerer med høy utvidelse tverrbindbare polydiorganosiloksanmasser, som oppnås ved blanding avoC,uj -dihydroksypolydiorganosiloksaner, ot. , w -bis-(triorganylsiloksy)-polyorgano-siloksaner, fyllstoffer og eventuelt pigmenter, titansyreestre. samt, som tverrbindingsmiddel, organyltrimetoksysilaner, hvorved. , det som fyllstoff anvendes utfelte, hydrofoberte kritt med en restfuktighet på under 0,4 vekt-?o.Anvendelse av massene som belegningsstoffer og fugetetnings-. masser.! Relieves exclusion of moisture storable and at ambient temperature under the influence of water or atmospheric air to high expansion stretch elastomers crosslinkable polydiorganosiloxane masses, which are obtained by mixing avoC, uj -dihydroxypolydiorganosiloxanes, etc. , w -bis- (triorganylsiloxy) -polyorgano-siloxanes, fillers and optionally pigments, titanium acid esters. and, as a crosslinking agent, organyltrimethoxysilanes, whereby. Precipitated hydrophobicized chalk with a residual moisture content of less than 0.4% by weight is used as filler. Use of the compositions as coatings and sealants masses.
Description
Foreliggende oppfinnelse angår et nøytralt, lagringsstabilt enkomponentsystem på basis av silikon og som tverrbinder ved atmosfærisk luft og som inneholder et organyltrimetoksysilan som tverrbindingsmiddel. The present invention relates to a neutral, storage-stable one-component system based on silicone which cross-links in atmospheric air and which contains an organyltrimethoxysilane as cross-linking agent.
Silikonpastaer som tverrbinder i atmosfærisk luft består som regel av cx ,co-dihydroksypolydiorganosiloksaner, silikonoljer , fyllstoffer og eventuelt pigmenter som blandes grundig med hverandre. Hvis man til slike pastaer setter organosilåner som inneholder mer enn to reaktive grupper og som reagerer både med silanolgruppene og med fuktig luft - hvorved disse reaksjoner erfaringsmessig katalyseres at katalysatorer som titan- og zirkonorganiske forbindelser samt tungmetallsalter - og utelukker man tilgang på vann eller vanndamp, oppstår det masser som herder først ved atmosfærisk luft. Slike systemer anvender for eksempel i bygningsbransjen for tetting av sanitær-, gulv- og veggfuger eller for tetting av vinduer mellom glass og ramme henholdsvis mellom ramme og vegg. Når det gjelder aluminiumsvinduer foretrekker man såkalte nøytrale systemer som for eksempel ikke spalter av eddiksyre eller andre karboksylsyrer og heller ingen aminer og som således ikke kan forårsake korrosjoner. Til disse nøytral-systemer hører blant annet alkoksysystemene, altså silikon-masser som som tverrbinder inneholder silaner med mer enn to alkoksygrupper. Således beskriver for eksempel DE-AS 1 118 454 systemer med OH-avsluttede polydiorganosiloksaner og silaner av typen Si(OR)4eller R'Si(0R)3, hvortil det settes tverrbindingskatalysatorer som organotinn- og organotitanforbindelser. Slike lK-alkoksysystemer er ikke lagringsstabile og tverrbinder allerede ved romtemperatur senest etter noen uker i pakningen. Silicone pastes that cross-link in atmospheric air usually consist of cx,co-dihydroxypolydiorganosiloxanes, silicone oils, fillers and possibly pigments that are mixed thoroughly with each other. If you add organosilanes to such pastes which contain more than two reactive groups and which react both with the silanol groups and with moist air - whereby these reactions are catalysed by experience that catalysts such as titanium and organic zirconium compounds as well as heavy metal salts - and you exclude access to water or water vapour, masses are formed which harden only in atmospheric air. Such systems are used, for example, in the construction industry for sealing sanitary, floor and wall joints or for sealing windows between glass and frame or between frame and wall. When it comes to aluminum windows, so-called neutral systems are preferred which, for example, do not split with acetic acid or other carboxylic acids and also no amines and which thus cannot cause corrosion. These neutral systems include, among other things, the alkoxy systems, i.e. silicone masses that contain silanes with more than two alkoxy groups as cross-linkers. Thus, for example, DE-AS 1 118 454 describes systems with OH-terminated polydiorganosiloxanes and silanes of the type Si(OR)4 or R'Si(OR)3, to which cross-linking catalysts such as organotin and organotitanium compounds are added. Such 1K-Alkoxy systems are not storage-stable and cross-link already at room temperature after a few weeks in the package at the latest.
Overraskende kan denne mangel settes til side ved hjelp av foreliggende oppfinnelse. Oppfinnelsen dreier seg herved om, under utelukkelse av fuktighet lagringsdyktige, ved omgivelsestemperatur under innvirkning av vann eller atmosfærisk luft, til rivfaste elastomer med høy utvidelse tverrbindbare polydiorganosiloksanmasser som kan oppnås ved blanding av cx fa>-dihydroksypolydiorganosiloksaner , a,u-bis-(triorganylsiloksy)-polyorganosiloksaner, fyllstoffer og eventuelt pigmenter, titansyreestre samt som tverrbindingsmiddel, organyltrimetoksysilaner,karakterisert vedat det som fyllstoff anvendes utfelt hydrofobert kritt med en restfuktighet på under 0,4 vekt-#. Surprisingly, this shortcoming can be set aside with the help of the present invention. The invention hereby concerns, subject to the exclusion of moisture, storable, at ambient temperature under the influence of water or atmospheric air, into tear-resistant elastomers with high expansion crosslinkable polydiorganosiloxane masses which can be obtained by mixing cxfa>-dihydroxypolydiorganosiloxanes, a,u-bis-(triorganylsiloxy )-polyorganosiloxanes, fillers and possibly pigments, titanium acid esters and as a cross-linking agent, organyltrimethoxysilanes, characterized in that precipitated hydrophobic chalk with a residual moisture of less than 0.4 wt-# is used as filler.
De således fremstilte pastaer er lagringsstabile ved romtemperatur langt over et halvt år, ved 50° C langt over 2 måneder, under utelukkelse av fuktighet. Silikonelastomerene som etter en slik lagring oppnås ved tverrbinding ved atmosfærisk luft har ikke mistet noen av sine gode mekaniske og andre egenskaper som påføringsforenelighet og vedhefting til de forskjelligste underlag. The pastes produced in this way are storage-stable at room temperature for well over half a year, at 50° C for well over 2 months, subject to the exclusion of moisture. The silicone elastomers which after such storage are obtained by cross-linking with atmospheric air have not lost any of their good mechanical and other properties such as application compatibility and adhesion to the most diverse substrates.
For fremstilling av oppfinnelsens RTV-lK-masser anvender man som polymer fortrinnsvis cx ,co-dihydroksypolydiorganosiloksaner som inneholder metylgrupper og hvis viskositet ved 20°C ligger mellom 1000 og 1 000 000 mPas, spesielt foretrukket mellom 10 000 og 300 000 mPas. Konsentrasjonen til polymerene bør ligge mellom 25 og 50 vekt-#. Den som mykningsolje foretrukne trimetylsiloksy-avsluttede polydimetylsiloksanolje med en viskositet mellom 30 og 10 000 mPas, målt ved 20° C, bør kun benyttes i den mengde som er nødvendig for inn-arbeiding av fyllstoffene i polymeren. For the production of the RTV-IK compounds of the invention, the polymer preferably used is cx,co-dihydroxypolydiorganosiloxanes which contain methyl groups and whose viscosity at 20°C is between 1000 and 1,000,000 mPas, particularly preferably between 10,000 and 300,000 mPas. The concentration of the polymers should be between 25 and 50% by weight. The preferred softening oil, trimethylsiloxy-terminated polydimethylsiloxane oil with a viscosity between 30 and 10,000 mPas, measured at 20° C, should only be used in the amount necessary for incorporating the fillers into the polymer.
Som optimale forsterkningsfyllstoffer skal spesielt nevnes utfelt og derved spesielt finoppdelte kritt med en midlere partikkelstørrelse under 0,5 pm og fortrinnsvis under 0,1 pm som er belagt med karboksylsyre som for eksempel stearinsyre eller silaner som for eksempel metyltriklorsilan og/eller dimetyldiklorsilan, og som derved er hydrofobert. Spesielt foretrukket er stearinsyre, hvis konsentrasjon bør ligge over 2,0 vekt-$, forutsatt en jevn fordeling. For fremstillingen av hvitfarvede tilsetningsstoffer bør man også anvende et kritt med høyest mulig hvithetsgrad og lavt farvestikk. As optimal reinforcing fillers, special mention should be made of precipitated and thereby especially finely divided chalk with an average particle size below 0.5 pm and preferably below 0.1 pm which is coated with carboxylic acid such as stearic acid or silanes such as methyltrichlorosilane and/or dimethyldichlorosilane, and which thereby being hydrophobic. Particularly preferred is stearic acid, the concentration of which should be above 2.0% by weight, assuming an even distribution. For the production of white-colored additives, you should also use a chalk with the highest possible degree of whiteness and low color stickiness.
For å oppnå holdfaste masser trenger man mellom 30 og 60 vekt-* kritt, hvorved spesielt finfordelte kritt gir god lagringsstabilitet allerede fra 35 vekt-*, mens kritt med en midlere partikkelstørrelse på over 0,1 pm må tilsettes i mengder på opptil 60 vekt-*. Fastleggelsen av holdfastheten skjer i henhold til DIN 65 262, del 3 ved 23°C og 50* relativ luftfuktighet på en frisk pastapåføring på vertikal hunn. Etter 30 minutter hør en 1 cm tykk pasta ikke ha rent mer enn 1,5 mm nedover. Denne norm betegnes også som luftfartsnormen. To achieve stable masses, you need between 30 and 60 weight-* of chalk, whereby especially finely divided chalk gives good storage stability already from 35 weight-*, while chalk with an average particle size of over 0.1 pm must be added in quantities of up to 60 weight -*. The holding strength is determined according to DIN 65 262, part 3 at 23°C and 50* relative humidity on a fresh paste application on a vertical female. After 30 minutes, a 1 cm thick paste should not clean more than 1.5 mm downwards. This standard is also referred to as the aviation standard.
Restfuktigheten i krittet måles i henhold til DIN 53 198, metode A (tørkingstap 2 timer ved 105°C). For å garantere den ifølge oppfinnelsen påståtte lagringsstabilitet for silikon-pastaen må man sikre at fuktighetsinnholdet i krittet ligger under 0,4 vekt-*. Dette kan oppnås uten kompliserte ytterligere tørkeforholdsregler ved at det utfelte og hydrofoberte kritt etter tørking og hos produsenten øyeblikkelig pakkes i forpakninger med vanndampsperre. The residual moisture in the chalk is measured according to DIN 53 198, method A (drying loss 2 hours at 105°C). In order to guarantee the storage stability of the silicone paste claimed according to the invention, it must be ensured that the moisture content of the chalk is below 0.4 weight-*. This can be achieved without complicated additional drying measures by the precipitated and hydrophobicized chalk being immediately packed in packages with a water vapor barrier after drying and at the manufacturer.
En ytterligere og meget avgjørende bestanddel av oppfinnelsen er anvendelsen av organyltrimetoksysilan og fortrinnsvis metyltrimetoksysilan som tverrbindingsmiddel. Høyere alkoksysilaner som for eksempel metyltrietoksysilan og tetraetoksysilan forringer lagringsstabilitetstiden merkbart. Andelen av metyltrimetoksysilan i pastaen bør fortrinnsvis ligge mellom 2 og 4 vekt-* og aller helst mellom 2,5 og 3 vekt-* for å bevirke god vedhefting også etter lang lagringstid. A further and very decisive component of the invention is the use of organyltrimethoxysilane and preferably methyltrimethoxysilane as a cross-linking agent. Higher alkoxysilanes such as methyltriethoxysilane and tetraethoxysilane noticeably reduce the storage stability time. The proportion of methyltrimethoxysilane in the paste should preferably lie between 2 and 4 weight-* and most preferably between 2.5 and 3 weight-* to effect good adhesion even after a long storage time.
Som titansyreester kan anvendes titantetraalkylestre, dialkyltitandialkylestre og andre titanorganoestre slik de for eksempel er nevnt i DE-PS 1 258 087. Den foretrukne andel av titanorganiske forbindelser i pastaen utgjør mellom 0,5 og 2 vekt-* hvorved de lavere andeler rundt 0,5 vekt-* fører til høyere bruddutvidelsesverdier. Dog må man ved blandingen passe på en periodisk viskositetsforhøyelse i massene og en tilsvarende dimensjonering av blandingsaggregatet. As titanium acid esters, titanium tetraalkyl esters, dialkyl titanium dialkyl esters and other titanium organo esters can be used as, for example, they are mentioned in DE-PS 1 258 087. The preferred proportion of titanium organic compounds in the paste amounts to between 0.5 and 2 weight-* whereby the lower proportions are around 0.5 weight-* leads to higher fracture expansion values. However, when mixing, care must be taken to periodically increase the viscosity of the masses and a corresponding dimensioning of the mixing unit.
Ved valget av kritt kan man oppnå de ovenfor beskrevne holdfaste systemer. Holdfastheten bør ikke tilstrebes ved hjelp av tilsetning av pyrogene eller utfelte kiselsyrer da dette kun fører til en stramming av elastomeren, noe som vises i sammenligningseksempel 6. By choosing chalk, you can achieve the permanent systems described above. The holding strength should not be achieved by adding pyrogenic or precipitated silicic acids as this only leads to a tightening of the elastomer, which is shown in comparative example 6.
Et ytterligere spesielt trekk ved oppfinnelsen ligger i at ingen av de tverrbindingsakselererende tungmetallforbindelser som for eksempel tinnorganiske forbindelser, er nødvendige. Dette gir på den ene side fordelen av høy lagringsstabilitet for disse enkomponentsystemer, på den annen side krever huddannelsestiden for oppfinnelsens pasta (5 til 10 minutter under normbetingelser) og den problemfrie tverrbinding, ingen ytterligere forholdsregler. A further special feature of the invention lies in the fact that none of the cross-linking accelerating heavy metal compounds such as organotin compounds are necessary. This gives, on the one hand, the advantage of high storage stability for these one-component systems, on the other hand, the skin formation time of the paste of the invention (5 to 10 minutes under standard conditions) and the problem-free cross-linking, require no further precautions.
Ved de allerede nevnte anvendelsesmuligheter har oppfinnelsens tetnings- og belegningsmasser følgende fremragende egenskaper: Holdfaste, lagringsstabile pastaer; With the already mentioned application possibilities, the sealing and coating compounds of the invention have the following outstanding properties: Firm, storage-stable pastes;
høyrivfaste og høyutvidbare elastomerer; og highly tear-resistant and highly extensible elastomers; and
påføringsforenelige systemer.application compatible systems.
De mekaniske verdier for de nedenfor gitte eksempler baserer seg på DIN-norm 53 505 hva angår Shore A-heten) og DIN 53 504 når det gjelder normstaven. The mechanical values for the examples given below are based on DIN standard 53 505 regarding the Shore A) and DIN 53 504 regarding the standard rod.
Vedheftingen ble bestemt etter 7 dagers gjennomherding av et ca. 10 mm tykt tetningsmateriale under normklimabetingelser og deretter etter 1, 3 og 7 dager under vann på følgende underlag: plateglass, kakler (glasserte), eloksal, aluminium, V4A-stål, jern, sink, kobber, hård-PVC, polymetakrylatglass, polyetylen, polykarbonat, tre og betong. Overflatene til disse materialene ble avfettet før pastapåføringen. Den vilkårlige vedhefting blir så angitt prosentualt via summen av alle stoffer og de fire gjennomherdingstrinn. Adhesion was determined after 7 days of curing of an approx. 10 mm thick sealing material under standard climate conditions and then after 1, 3 and 7 days under water on the following substrates: plate glass, tiles (glazed), anodized, aluminium, V4A steel, iron, zinc, copper, hard PVC, polymethacrylate glass, polyethylene, polycarbonate, wood and concrete. The surfaces of these materials were degreased before the paste application. The arbitrary adhesion is then indicated as a percentage via the sum of all substances and the four through-hardening steps.
Utover dette prøvet man påføringsforeneligheten som følger: To treplater ble begge lakkert med hvit dekklakk på alkyd-harpiksbasis og med brun dekklakk som vandig emulsjon på akrylbasis. Etter gjennomherding av lakken ble den følgende dag begge treplater belagt med tetningsstoff og etter to uker prøvet ved skjæring og trekking hvorvidt tetningsstoffet heftet godt ved den lakkerte undergrunn. In addition to this, application compatibility was tested as follows: Two wooden panels were both painted with white topcoat on an alkyd resin base and with brown topcoat as an aqueous emulsion on an acrylic base. After the lacquer had fully hardened, the following day both wooden panels were coated with sealant and after two weeks it was tested by cutting and pulling whether the sealant adhered well to the varnished substrate.
Lagringsstabiliteten ble bestemt som glassvedhefting av elastomeren i uker lagringstid ved romtemperatur henholdsvis 50°C. The storage stability was determined as glass adhesion of the elastomer during weeks of storage time at room temperature or 50°C.
De angitte viskositeter gjelder 23°C.The specified viscosities apply at 23°C.
De følgende eksempler skal illustrere oppfinnelsens krevede RTV-lK-masser. The following examples shall illustrate the invention's required RTV-IK compounds.
Eksempel 1Example 1
I en blanding av 27,9 vektdeler a ,u-dihydroksypolydimetylsiloksan med viskositeten 50 000 mPas og 15,5 vektdeler a,to-bis-(tr imetylsi loksy )-polydimetylsiloksan med viskositet 1000 mPas røres det inn 51,0 vektdeler av et utfelt og med stearinsyre behandlet kritt med en midlere partikkeldiameter på 0,08 pm og et fuktighetsinnhold på 0,3 vekt-* i løpet av 30 minutter. Deretter tilsettes 2,0 vektdeler di-i-butoksytitandiacetateddiksyreetylesterchelat, det hele omrøres i 5 minutter og evakueres i 15 minutter til 2 mbar. Deretter innrøres også 3,6 vektdeler metyltrimetoksysilan og systemet røres i 15 minutter under vakuum med opptil 50 omdr./min. Massen fylles i pakninger og lagres under utelukkelse av fuktighet. In a mixture of 27.9 parts by weight of a,u-dihydroxypolydimethylsiloxane with a viscosity of 50,000 mPas and 15.5 parts by weight of a,to-bis-(trimethylsiloxy)-polydimethylsiloxane with a viscosity of 1,000 mPas, 51.0 parts by weight of a precipitate are stirred and stearic acid treated chalk with an average particle diameter of 0.08 pm and a moisture content of 0.3 wt-* within 30 minutes. Then 2.0 parts by weight of di-i-butoxytitanium diacetate acetic acid ethyl ester chelate are added, the whole is stirred for 5 minutes and evacuated for 15 minutes at 2 mbar. Then 3.6 parts by weight of methyltrimethoxysilane are also stirred in and the system is stirred for 15 minutes under vacuum at up to 50 rpm. The pulp is filled into packages and stored under the exclusion of moisture.
Pastaen vulkaniseres under innvirkning av luftfuktighet (normklima: 23°C, 50* relativ fuktighet) til en silikonelastomer med følgende egenskaper: The paste is vulcanized under the influence of atmospheric humidity (standard climate: 23°C, 50* relative humidity) into a silicone elastomer with the following properties:
Eksempel 2 Example 2
36,5 vektdeler cx ,u-dihydroksypolydimetylsiloksan med viskositet 50 000 mPas og 14,5 vektdeler a ,to ,bis-( trimetylsiloksy)-polydimetylsiloksan med viskositet 100 mPas hiandes med 44,0 vektdeler av et utfelt og belagt kritt med et fuktighetsinnhold på 0,3 vekt-* som i eksempel 1. I denne blanding innrøres etter hverandre 1,5 vektdeler di-i-butoksytitandiacetateddiksyreetylesterchelat og 3,5 vektdeler metyltrimetoksysilan i løpet av 5 minutter og det hele evakueres som i 15 minutter ved 2 mbar. Pastaen fylles i beholdere under utelukkelse av luftfuktighet og lagres. 36.5 parts by weight of cx,u-dihydroxypolydimethylsiloxane with a viscosity of 50,000 mPas and 14.5 parts by weight of a,to,bis-(trimethylsiloxy)-polydimethylsiloxane with a viscosity of 100 mPas are combined with 44.0 parts by weight of a precipitated and coated chalk with a moisture content of 0.3 weight-* as in example 1. Into this mixture, 1.5 parts by weight of di-i-butoxytitanium diacetate acetic acid ethyl ester chelate and 3.5 parts by weight of methyltrimethoxysilane are stirred one after the other over the course of 5 minutes and the whole is evacuated as for 15 minutes at 2 mbar. The paste is filled into containers under the exclusion of humidity and stored.
Egenskaper til den gjennomherdede silikonelastomer: Properties of the fully cured silicone elastomer:
Eksempel 3 Example 3
40,5 vektdeler cx ,G)-dihydroksypolydimetylsiloksan med viskositet 150 000 mPas og 14,0 vektdeler cx ,co-bis-( trimetyl-slloksy)-polydimetylsiloksan med viskositet 100 mPas blandes med 40 vektdeler utfelt og belagt kritt med et fuktighetsinnhold på 0,3 vekt-* som i eksempel 1 og 2 og analogt de tidligere eksempler innrøres etter hverandre 2,5 vektdeler di-i-butoksytitandiacetateddiksyreetylesterchelat og 3,0 vektdeler metyltrimetoksysilan i 5 minutter hvoretter det hele evakueres i 15 minutter til 2 mbar. Pastaen fylles og lagres under utelukkelse av fuktighet. 40.5 parts by weight cx ,G)-dihydroxypolydimethylsiloxane with a viscosity of 150,000 mPas and 14.0 parts by weight of cx ,co-bis-(trimethyl-sloxy)-polydimethylsiloxane with a viscosity of 100 mPas are mixed with 40 parts by weight of precipitated and coated chalk with a moisture content of 0 .3 weight-* as in examples 1 and 2 and analogously to the previous examples, 2.5 parts by weight of di-i-butoxytitanium diacetate acetic acid ethyl ester chelate and 3.0 parts by weight of methyltrimethoxysilane are stirred in for 5 minutes, after which the whole is evacuated for 15 minutes to 2 mbar. The pasta is filled and stored under the exclusion of moisture.
Egenskaper til den gjennomherdede silikonelastomer: Properties of the fully cured silicone elastomer:
Eksempel 4 Example 4
40,5 vektdeler cx ,(i)-dihydroksypolydimetylsiloksan med viskositet 50 000 mPas, 16,0 vektdeler cx ,o)-bis-(trimetylsiloksy)-polydimetylsiloksan med viskositet 100 mPas, 40 vektdeler utfelt og belagt kritt med et fuktighetsinnhold på 40.5 parts by weight cx ,(i)-dihydroxypolydimethylsiloxane with a viscosity of 50,000 mPas, 16.0 parts by weight of cx ,o)-bis-(trimethylsiloxy)-polydimethylsiloxane with a viscosity of 100 mPas, 40 parts by weight of precipitated and coated chalk with a moisture content of
0,3 vekt-*, 1,0 vektdeler di-i-butoksytitandiacetateddiksyreetylesterchelat og 2,5 vektdeler metyltrimetoksysilan blandes og fylles på beholdere og lagres som i de ovenfor gitte eksempler. 0.3 parts by weight, 1.0 parts by weight of di-i-butoxytitanium diacetate acetic acid ethyl ester chelate and 2.5 parts by weight of methyltrimethoxysilane are mixed and filled into containers and stored as in the examples given above.
Egenskaper til den gjennomherdede silikonelastomer: Properties of the fully cured silicone elastomer:
Eksempel 5 Example 5
39,0 vektdeler cx ,co-dihydroksypolydimetylsiloksan med viskositet 50 000 mPas og 11,0 vektdeler cx ,oj-bis-( trimetylsiloksy )-polydimetylsiloksan med viskositet 100 mPas, 47,0 vektdeler utfelt og belagt kritt med et fuktighetsinnhold på 0,25 vekt-* blandes som i de tidligere eksempler hvoretter 2,0 vektdeler metyltrimetoksysilan innrøres i 5 minutter og det hele evakueres i 15 minutter til 2 mbar. I denne blanding innrøres 1,0 vektdeler av de følgende titanorganiske forbindelser i 5 minutter hvoretter det hele evakueres i 15 minutter til 2 mbar: 39.0 parts by weight of cx ,co-dihydroxypolydimethylsiloxane with a viscosity of 50,000 mPas and 11.0 parts by weight of cx ,oj-bis-(trimethylsiloxy)-polydimethylsiloxane with a viscosity of 100 mPas, 47.0 parts by weight of precipitated and coated chalk with a moisture content of 0.25 weight-* is mixed as in the previous examples, after which 2.0 parts by weight of methyltrimethoxysilane are stirred in for 5 minutes and the whole is evacuated for 15 minutes to 2 mbar. In this mixture, 1.0 parts by weight of the following organic titanium compounds are stirred for 5 minutes, after which the whole is evacuated for 15 minutes to 2 mbar:
5.1 Tetrakis-2-etylheksyltitånat,5.1 Tetrakis-2-ethylhexyl titanate,
5.2 Titantetrabutylat,5.2 Titanium tetrabutylate,
5.3 Titantetraetylat.5.3 Titanium tetraethylate.
Pastaen ble i hvert tilfelle fylt i pakninger og lagret under utelukkelse av luftfuktighet. In each case, the pasta was filled in packages and stored under the exclusion of atmospheric humidity.
Sammenlignlngseksempel 6 Comparative example 6
39,0 vektdeler cx ,o)-dihydroksypolydimetylsiloksan med viskositet 50 000 mPas, 13,5 vektdeler cx ,u)-bis-( trimetylsiloksy)-polydlmetylsiloksan med viskositet 100 mPas, 43,0 vektdeler utfelt og belagt kritt med et fuktighetsinnhold på 0,25 vekt-* blandes som i de tidligere eksempler; deretter innrøres i rekkefølge 1 vektdel di-i-butoksytitandiacetateddiksyreetylesterchelat, 2,5 vektdeler metyltrimetoksysilan og 1,5 vektdeler pyrogen, siloksanfylt kiselsyre med en spesifikk overflate på 120 m<2>/g og et fuktighetsinnhold på under 0,5 vekt-* i 5 minutter hvoretter det hele i hvert tilfelle evakueres i 15 minutter til 2 mbar. Pastaen fylles og lagres i beholdere under utelukkelse av fuktighet. 39.0 parts by weight cx,o)-dihydroxypolydimethylsiloxane with a viscosity of 50,000 mPas, 13.5 parts by weight of cx,u)-bis-(trimethylsiloxy)-polydlmethylsiloxane with a viscosity of 100 mPas, 43.0 parts by weight of precipitated and coated chalk with a moisture content of 0 .25 weight-* is mixed as in the previous examples; then 1 part by weight of di-i-butoxytitanium diacetate acetic acid ethyl ester chelate, 2.5 parts by weight of methyltrimethoxysilane and 1.5 parts by weight of pyrogenic, siloxane-filled silicic acid with a specific surface area of 120 m<2>/g and a moisture content of less than 0.5 weight-* in 5 minutes, after which the whole in each case is evacuated for 15 minutes to 2 mbar. The pasta is filled and stored in containers under the exclusion of moisture.
Mekaniske egenskaper for den gjennomherdede silikonelastomer: Mechanical properties of the fully cured silicone elastomer:
SammenlIgnlngseksempel 7 Comparison example 7
Man fremstiller en pasta som i eksempel 4, men med den forskjell at man tilsetter utfelte, belagte kritt med et fuktighetsinnhold på 1,2 vekt-* (forårsaket ved lagring i atmosfærisk luft). A paste is prepared as in example 4, but with the difference that precipitated, coated chalk is added with a moisture content of 1.2 weight-* (caused by storage in atmospheric air).
Den således oppnådde pasta er riktignok holdfast (luftfarts-norm 1 mm), dog fornetter den allerede etter en ukes lagring ved 50°C i pakningen. The paste obtained in this way is indeed durable (aviation standard 1 mm), however, it cross-links already after one week of storage at 50°C in the packaging.
Claims (10)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE3839034A DE3839034A1 (en) | 1988-11-18 | 1988-11-18 | UNDER HUMIDITY EXCLUSION STORAGE-RANGING RTV-1K MASSES |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| NO894361D0 NO894361D0 (en) | 1989-11-02 |
| NO894361L true NO894361L (en) | 1990-05-21 |
Family
ID=6367431
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| NO89894361A NO894361L (en) | 1988-11-18 | 1989-11-02 | DURABLE STORAGE STABLE RTV-1K MASSES. |
Country Status (8)
| Country | Link |
|---|---|
| EP (1) | EP0369291A2 (en) |
| JP (1) | JPH02189365A (en) |
| KR (1) | KR900007966A (en) |
| AU (1) | AU4434289A (en) |
| CA (1) | CA2003089A1 (en) |
| DE (1) | DE3839034A1 (en) |
| FI (1) | FI895458A0 (en) |
| NO (1) | NO894361L (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5053442A (en) * | 1990-01-16 | 1991-10-01 | Dow Corning Corporation | Low modulus silicone sealants |
| US5051455A (en) * | 1990-01-16 | 1991-09-24 | Dow Corning Corporation | Adhesion of silicone sealants |
| US5432007A (en) * | 1992-10-06 | 1995-07-11 | Shizu Naito | Solvent-free organosiloxane composition and its use |
| EP0649879A3 (en) * | 1993-10-26 | 1995-10-04 | Dow Corning | High tear strength silicone compositions. |
| GB201103689D0 (en) * | 2011-03-04 | 2011-04-20 | Dow Corning | Organosil oxane compositions |
-
1988
- 1988-11-18 DE DE3839034A patent/DE3839034A1/en not_active Withdrawn
-
1989
- 1989-11-02 NO NO89894361A patent/NO894361L/en unknown
- 1989-11-02 AU AU44342/89A patent/AU4434289A/en not_active Abandoned
- 1989-11-07 EP EP89120574A patent/EP0369291A2/en not_active Withdrawn
- 1989-11-13 JP JP1292512A patent/JPH02189365A/en active Pending
- 1989-11-16 KR KR1019890016582A patent/KR900007966A/en not_active Application Discontinuation
- 1989-11-16 CA CA002003089A patent/CA2003089A1/en not_active Abandoned
- 1989-11-16 FI FI895458A patent/FI895458A0/en not_active Application Discontinuation
Also Published As
| Publication number | Publication date |
|---|---|
| FI895458A0 (en) | 1989-11-16 |
| DE3839034A1 (en) | 1990-05-23 |
| CA2003089A1 (en) | 1990-05-18 |
| KR900007966A (en) | 1990-06-02 |
| JPH02189365A (en) | 1990-07-25 |
| EP0369291A2 (en) | 1990-05-23 |
| AU4434289A (en) | 1990-05-24 |
| NO894361D0 (en) | 1989-11-02 |
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