HK1142351B - Architectural unit possessing rapid deep-section cure silicone rubber component - Google Patents
Architectural unit possessing rapid deep-section cure silicone rubber component Download PDFInfo
- Publication number
- HK1142351B HK1142351B HK10108786.9A HK10108786A HK1142351B HK 1142351 B HK1142351 B HK 1142351B HK 10108786 A HK10108786 A HK 10108786A HK 1142351 B HK1142351 B HK 1142351B
- Authority
- HK
- Hong Kong
- Prior art keywords
- amount
- weight percent
- bis
- component
- total composition
- Prior art date
Links
Description
Technical Field
The present invention relates to a building element having at least two components bonded together with a rapidly formed silicone rubber composition having strength and deep-section cure.
Background
Skyscrapers and "high-rise" construction projects of the construction industry are rapidly evolving, especially in developing economies. The industry uses sealants to bond various building materials (e.g., glass windows and metals) together. By its nature, such construction is carried out at high altitudes, and therefore, special sealant properties are necessary for this market. These properties include ease of application and very rapid development of strength and deep-section cure. Conventional sealants provide ease of application, e.g., one-part sealants. However, conventional silicone polymer systems typically develop strength and deep-section cure rather slowly, i.e., after several days to several weeks of exposure to humid air.
Moreover, rapid development of strength and deep-section cure is often desirable in certain sealant and/or adhesive applications (e.g., "high-rise" construction, automotive, and insulating glass applications).
There remains a need in the art for silicone sealants that develop rapidly (i.e., hours to days) with strength and deep-section cure.
Drawings
FIG. 1 is a cross-sectional side view of an Insulated Glass Unit (IGU) maintained in sealed relation with a deep-section fast-setting glazing composition (glass composition) according to the invention.
FIG. 2 is a bird's eye view cross-section of the exterior of a "high-rise" building illustrating a plurality of installed window systems including the IGU of FIG. 1.
FIG. 3 is a graphical representation of the "tack free time" of comparative examples 1 and 2 and examples 1 and 2.
FIG. 4 is a graphical representation of the "deep-section cure" rates for example 1 and comparative example 1.
FIG. 5 is a graphical representation of the "deep-section cure" rates for example 2 and comparative example 2.
Disclosure of Invention
The present invention provides a construction element having at least two components bonded together or otherwise maintained in sealed relationship to one another with a silicone rubber composition obtained by curing a mixture comprising:
a) at least one silanol-terminated diorganopolysiloxane (diorganopolysiloxane);
b) at least one crosslinker for the one or more silanol terminated diorganopolysiloxanes;
c) at least one catalyst for the crosslinking reaction;
d) a deep-section rapidly solidified amount of zinc oxide; and
e) optionally at least one additional component selected from: alkyl-terminated diorganopolysiloxane, filler, uv stabilizer, antioxidant, tackifier, cure accelerator, thixotropic agent, plasticizer, moisture scavenger, pigment, dye, surfactant, solvent, and antimicrobial agent.
Detailed Description
The expression "building element" as used herein denotes a prefabricated or manufactured unit for use in building a building, such as a window (specifically, an insulated glass unit ("IGU")), a glazed door, a door containing one or more windows, a prefabricated window, a sliding door having one or more windows, a folding door having one or more windows, a curtain wall, shop glass (shop glazing), structural glazing (structural glazing), skylight, and light fixtures (light fixtures), and the like, wherein the glass is bonded to the building element-containing structural element using a bonding, glazing, sealing, caulking or adhesive composition.
The term "glass" is used herein in its ordinary sense and includes glass and glass substitutes such as polyacrylates (especially polymethylmethacrylate) and polycarbonates and the like (including but not limited to various transparent, translucent and opaque glasses).
The expression "glazing composition" and the terms "adhesive composition", "bonding composition", "sealing composition" or "caulking composition" as used herein includes or comprises the silicone rubber-formed composition of the present invention.
As used herein, a structural element is a material used in the construction of, for example, buildings, window frames and window frame assemblies, and the like, which is manufactured from materials known in the art (e.g., wood, stone, brick, steel, aluminum, brass, iron, copper, concrete, plastic-covered wood or metal, and the like).
As used herein, the term "compatible" means that the optional component does not materially negatively or adversely affect the storage stability of the part containing the optional component and that the intended function of the optional component is not materially negatively or adversely affected when contained in the part.
As understood herein, curing of the sealing composition may be expressed as "tack-free time" or surface cure and "deep-section cure" or cure along the thickness of the sealant. Tack free time was tested by the following method: the sealant was spread to the desired thickness (e.g., 6.35mm) on a Teflon mold and a 10g Stainless Steel (SS) weight was placed on the sealant at various time intervals. The tack-free time is the time during which no substance sticks to the surface of the weight. Alternatively, the "deep-section cure" or through-thickness cure is tested based on periodically cutting the spread material through the thickness to detect full cure. The time taken for the material to fully cure through the thickness is referred to as the deep-section cure time, also referred to as the "thickness-section cure time". In addition to visual inspection, the inventors have devised a method of measuring deep-section cure by extracting uncured material of the sealant with a solvent (described in more detail below).
Referring to fig. 1, an insulated glass unit 10 includes glass sheets 1 and 2 maintained in spaced apart relation using a gas seal assembly having a first gas seal member 4, a continuous spacer member 5, and a second sealant 7. The space 6 between sheets 1 and 2 is filled with one or more insulating gases such as argon. A deep-section fast-cure glazing composition 8 prepared as described below was placed between glass sheet 1 and window frame assembly 9. Glass sheets 1 and 2 can be made of any of a variety of materials, such as glass (e.g., clear float glass, annealed glass, tempered glass, brown glass, tinted glass, such as low energy glass (low energy glass), etc.), acrylic, polycarbonate, etc.
The use of the deep-section cure bedding glaze composition 8 (i.e., the silicone rubber-forming composition of the present invention) in the aforementioned insulating glass units improves productivity in the manufacture of these units with improved adhesion development and rapid formation of strength and deep-section cure. In addition to providing the performance attributes required for typical glazing sealants, including adhesion, bond strength, and elongation, other benefits include long shelf life and improved application rates of the sealant. As a result, the deep-section cured bedding glaze composition 8 is useful as a sealant and/or adhesive because it exhibits high adhesive strength (including a good balance between shear adhesive strength and peel adhesive strength) and is therefore particularly suitable for use as a glazing sealant in the manufacture of various glazing units, such as glazing units in high-rise buildings.
The first sealing member 4 of the insulating glass unit 10 may be composed of polymeric materials known in the art, for example, rubber-based materials such as polyisobutylene, butyl rubber, polysulfide, EPDM rubber, nitrile rubber, and the like. Other useful materials include polyisobutylene/polyisoprene copolymers, polyisobutylene polymers, brominated olefin polymers, copolymers of polyisobutylene and para-methylstyrene, copolymers of polyisobutylene and brominated para-methylstyrene, butyl rubber-copolymers of isobutylene and isoprene, ethylene-propylene polymers, polysulfide polymers, polyurethane polymers, styrene butadiene polymers, and the like.
As described above, the first gas sealing member 4 may be made of a material having very good sealing properties, such as polyisobutylene. A desiccant may be included in continuous spacing member 5 to remove moisture from the insulating gas-filled space between glass sheets 1 and 2. Useful desiccants are those that do not absorb the insulating gas or gases that fill the interior of the insulating glass unit.
As described more fully below, the deep-section cure bedding glaze composition 8 of the present invention is a stable room temperature curable silicone sealant composition that provides rapid primerless bond strength and deep-section cure.
The deep-section cure bedding glaze composition 8 of the present invention is comprised of a Room Temperature Vulcanizing (RTV) silicone rubber-forming composition. A general description of each component of the deep-section fast-curing glazing composition is given below:
the silanol terminated diorganopolysiloxane polymer (SDPS), component (a), of the deep-section cure bedding glaze composition 8 of the present invention is advantageously selected from the group of materials having the general formula:
MaDbD′c
and subscript a ═ 2, b equal to or greater than 1, and subscript c is 0 or a positive number, where
M=(HO)3-x-yR1 xR2 ySiO1/2;
And subscript x is 0, 1 or 2, subscript y is 0 or 1, and subject to the following limitations: x + y is less than or equal to 2, wherein R1And R2Independently selected from monovalent hydrocarbon radicals having up to about 60 carbon atoms; wherein
D=R3R4SiO2/2;
Wherein R is3And R4Independently selected from monovalent hydrocarbon radicals having up to about 60 carbon atoms; wherein
D′=R5R6SiO2/2;
Wherein R is5And R6Independently selected from monovalent hydrocarbon radicals having up to about 60 carbon atoms.
In one embodiment of the invention, the incorporation level of the diorganopolysiloxane wherein the silicon atom at each polymer chain end is silanol terminated ranges from about 5 weight percent to about 95 weight percent of the total composition, in another embodiment from about 20 weight percent to about 85 weight percent of the total composition, and in yet another embodiment from about 30 weight percent to about 60 weight percent of the total composition.
Suitable cross-linking agents, component (b), for use in the deep-section cure bedding glaze composition 8 of the present invention include alkyl silicates having the general formula:
(R7O)(R8O)(R9O)(R10O)Si
wherein R is7、R8、R9And R10Independently selected from monovalent C1To C60A hydrocarbyl group.
Other suitable crosslinking agents include, but are not limited to, tetra-N-propylsilicate (NPS), tetraethylorthosilicate, and methyltrimethoxysilane (MTMS), Vinyltrimethoxysilane (VTMS), and similar alkyl-substituted alkoxysilane compositions, and the like.
In one embodiment of the invention, the level of incorporation of the alkyl silicate (crosslinker) is from about 0.1 wt.% to about 10 wt.% of the total composition. In another embodiment of the invention, the level of incorporation of the alkyl silicate (crosslinker) is from about 0.3 wt.% to about 5 wt.% of the total composition. In yet another embodiment of the present invention, the level of incorporation of the alkyl silicate (crosslinker) is from about 0.5 wt.% to about 1.5 wt.% of the total composition.
A suitable catalyst for use in the deep-section cure bedding glaze composition 8 of the present invention, component (c), may be any catalyst known to be useful in promoting crosslinking in silicone sealant compositions. The catalyst may include a metal catalyst and a non-metal catalyst. Examples of the metal portion of the metal condensation catalyst useful in the present invention include tin, titanium, zirconium, lead, iron, cobalt, antimony, manganese, bismuth and zinc compounds.
According to one embodiment of the present invention, tin compounds useful for promoting crosslinking in silicone sealing compositions include: such as dibutyltin dilaurate, dibutyltin diacetate, dibutyltin dimethoxide, tin octoate, isobutyltin tricerate, dibutyltin oxide, solubilized dibutyltin oxide, dibutyltin bis (diisooctylphthalate), bis (tripropoxysilyl) dioctyltin, dibutyltin bis (acetylacetonate), tin compounds such as silylated dibutyltin dioxide (silylated dibutyltin dioxide), tris (suberic acid) methoxycarbonylphenyl tin (carbomethoxyphenyl tin tris-uberate), isobutyltin triscalate, dimethyltin dibutyrate, dimethyltin dineodecanoate, triethyltin tartrate, dibutyltin dibenzoate, tin oleate, tin naphthenate, butyltin tris (2-ethylhexylhexanoate), butyltin butyrate (butyltitanate) and tin butyrate (tinbutryrate).
In one embodiment of the invention, the catalyst is a metal catalyst. In another embodiment of the invention, the metal catalyst is selected from tin compounds, and in yet another embodiment of the invention, the metal catalyst is solubilized dibutyltin oxide.
According to another embodiment of the present invention, titanium compounds useful for promoting crosslinking in silicone sealing compositions include: bis (isopropoxy) Titanium bis (ethylacetoacetate) (di (isopropoxide)) Titanium bis (ethylacetoacetate) [ Dupont; tyzor DC ]; bis (isobutoxy) bis (ethylacetoacetate) titanium (di (isobutoxide) titanomabis (ethyl acetate) [ Johnson Matthey; vertec KE6 ]; di (n-butoxy) bis (ethylacetoacetate) Titanium (Di (n-butoxide) Titanium bis (ethylacetoacetate)) [ johnson matthey ]; bis (ethylacetoacetate) 1, 3-propylenedioxytitanium (1, 3-propanediol) salts; titanium isopropoxide (triethanolamine) isopopoxide [ Dupont; tyzor TE ]; bis (methyl diglycolate) bis (triethanolamino) titanium (bis (triethanolamino) titanium di (methyl iglycolate)) [ Sanmar; isocat ETAM ]; diisopropoxy (bis-2, 4-pentanedionate) titanium (titanyldiisoproxide) (bis-2, 4-pentanedionate)) [ Dupont; tyzor AA ]; ethoxyisopropoxybis (2, 4-pentanedionato) Titanium (Titanium ethoxide isopopoxidibis- (2, 4-pentanedionate)) [ Sanmar; isocat AA 65 ]; bis (2, 4-pentanedione) (2-EHA) Titanium (Titanium bis- (2, 4-pentanedionate) (2-EHA (2-ethylhexyl acrylate))) [ johnson matthey; vertec XL100 ]; and tetraalkyl titanates (e.g., tetra-n-butyl titanate and tetra-isopropyl titanate), and the like.
According to one embodiment of the invention, the catalyst used for the crosslinking reaction is titanium bis (isopropoxide) bis (ethylacetoacetate).
In one embodiment of the invention, the level of incorporation of the catalyst is from about 0.001% to about 1% by weight of the total composition. In another embodiment of the invention, the level of incorporation of the catalyst is from about 0.003 wt% to about 0.5 wt% of the total composition. In yet another embodiment of the present invention, the level of incorporation of the catalyst is from about 0.005 wt.% to about 0.2 wt.% of the total composition.
The deep-section cure bedding glaze composition 8 of the present invention provides a room temperature curable silicone sealant composition that cures to provide rapid deep-section cure. The rapid deep-section cure is provided by particulate zinc oxide (d) present in the room temperature curable silicone sealing composition in at least about 1 part by weight per 100 parts by weight of the total composition of the room temperature curable silicone sealing composition. In one embodiment of the invention, the zinc oxide is present in an amount of from about 2 to about 30 parts by weight per 100 parts by weight of the total composition, and in another embodiment from about 5 to about 20 parts by weight per 100 parts by weight of the total composition.
The particulate zinc oxide (d) of the present invention has an average particle size of less than about 1 micron, from about 50 to about 70nm, and from about 5 to about 30m2Surface area in g. The zinc oxide (d) has a purity of about 80 to about 99.9% and a pH of about 7.0 to about 9.0. The zinc oxide of the present invention may be available as White Seal (IP 100) (available from MLA group of Industries, Kanpur, India); zincosil NK-T-150 (available from MLagroup of Industries, Kanpur, India); zincosil AH-90 (available from MLA group of industries, Kanpur, India); ACS (available from Aldrich Chemical Co.); zinc oxide Nano powder (available from Aldrich Chemical C)o.) commercially available.
According to one embodiment of the present invention, the deep-section cure bedding glaze composition 8 is obtained as a "one-component" composition (wherein all the ingredients are contained in one package) that cures when exposed to atmospheric air.
According to another embodiment of the present invention, a "two-component" composition (which is well known in the art) is used to obtain the deep-section cure bedding glaze composition 8. In a two-component system, the first component comprises a polydiorganosiloxane as described herein and zinc oxide, and the second component comprises a crosslinker such as the crosslinker described herein above. The second component may also contain certain fillers and curing catalysts for room temperature curable silicone compositions. The particulate zinc oxide may be added to either the first or second component. The "components" of these two-component compositions are stored in separate packages to prevent premature curing (which can occur if all the ingredients are mixed for too long before the composition is used).
According to one embodiment of the present invention, the deep-section cure bedding glaze composition 8 of the present invention further comprises an alkoxysilane or blend of alkoxysilanes as an adhesion promoter. In one embodiment, the adhesion promoter may be a combination blend of N-2-aminoethyl-3-aminopropyltrimethoxysilane and 1, 3, 5-tris (trimethoxysilylpropyl) isocyanurate. Other adhesion promoters that may be used in the present invention include, but are not limited to, N-2-aminoethyl-3-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, bis (gamma-trimethoxysilylpropyl) amine, N-phenyl-gamma-aminopropyltrimethoxysilane, triaminofunctionalized trimethoxysilane (triaminofunctionalized trimethoxysilane), gamma-aminopropylmethyldiethoxysilane, methacryloxypropyltrimethoxysilane, methylaminopropyltrimethoxysilane, gamma-glycidoxypropylethyldimethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-glycidoxyethyltrimethoxysilane (gamma-glycidoxytrimethyltriethoxysilane), Beta- (3, 4-epoxycyclohexyl) propyltrimethoxysilane, beta- (3, 4-epoxycyclohexyl) ethylmethyldimethoxysilane, isocyanatopropyltriethoxysilane (isocyatrophopylidyne), isocyanatopropylmethyldimethoxysilane, beta-cyanoethyltrimethoxysilane, gamma-acryloxypropyltrimethoxysilane, gamma-methacryloxypropylmethyldimethoxysilane, 4-amino-3, 3-dimethylbutyltrimethoxysilane and N-ethyl-3-trimethoxysilyl-2-methylpropylamine, and the like.
The alkoxysilane (adhesion promoter) has an incorporation level of about 0.1 wt.% to about 20 wt.%. In one embodiment of the invention, the tackifier is about 0.3 wt% to about 10 wt% of the total composition. In another embodiment of the invention, the tackifier is about 0.5 wt% to about 2 wt% of the total composition.
In one embodiment, the deep-section cured bedding glaze composition 8 of the present invention includes a plasticizer to reduce the modulus of the cured elastomer. The plasticizer may be a polydimethylsiloxane having terminal triorganosiloxy units (terminal triorganosiloxy units) wherein the organic groups are methyl, vinyl or phenyl groups, or a combination of these groups. For example, polydimethylsiloxanes used as plasticizers or modulus reducers may typically have viscosities of from 100 to 100,000 mpa-s (measured at 25 ℃), and may be used in amounts of up to 80 parts by weight per 100 parts by weight of polymeric material.
The deep-section cure bedding glaze composition 8 of the present invention may also include a filler. Suitable fillers for the present invention include, but are not limited to, ground, precipitated and colloidal calcium carbonate treated with compounds such as stearates or stearic acid; reinforcing silicas such as fumed silica, precipitated silica, silica gels, and hydrophobized silica and silica gels; crushed and ground quartz, alumina, aluminium hydroxide, titanium hydroxide, diatomaceous earth, iron oxide, carbon black and graphite or clays such as kaolin, bentonite or montmorillonite, talc and mica, etc.
In one embodiment of the invention, the filler is a calcium carbonate filler, a silica filler or a mixture thereof. In another embodiment of the present invention, zinc oxide (d) is added directly to the filler. The type and amount of filler added depends on the physical properties desired for the cured silicone composition. In another embodiment of the invention, the amount of filler is from 0 to about 90 weight percent of the total composition. In yet another embodiment of the present invention, the amount of filler is from about 5% to about 60% by weight of the total composition. In yet another embodiment of the present invention, the amount of filler is from about 10 to about 40 weight percent of the total composition. The filler may be a single substance or a mixture of two or more substances.
The deep-section cure bedding glaze composition 8 of the present invention may optionally comprise a nonionic surfactant compound selected from the group consisting of: the amount of the nonionic surfactant compound is slightly above 0% to about 10%, more preferably from about 0.1% to about 5%, and most preferably from about 0.5% to about 0.75% by weight based on the total composition of polyethylene glycol, polypropylene glycol, ethoxylated castor oil, oleic acid ethoxylate, alkylphenol ethoxylate, copolymers of Ethylene Oxide (EO) and Propylene Oxide (PO) and copolymers of silicones and polyethers (silicone polyether copolymers), copolymers of ethylene oxide and propylene oxide and copolymers of silicones, and mixtures thereof.
The deep-section cure bedding glaze composition 8 of the present invention may be prepared using other ingredients such as colorants and pigments conventionally used in Room Temperature Vulcanizing (RTV) silicone compositions, so long as they do not interfere with the desired properties.
The following non-limiting example illustrates a deep-section cured bedding glaze composition 8 of the present invention:
comparative examples 1 and 2 preparation of sealing formulations:
TABLE 1
| Material | Amount in grams (g) |
| Silanol (30000cst) | 34 |
| OMYACARB FT-CaCO3 | 50 |
| ZnO | 0 |
| Secondary treated fumed silica | 6 |
| Dimethyl polysiloxane plasticizer | 10 |
Comparative examples 1 and 2 were prepared in the absence of zinc oxide and consisted of the various ingredients shown in table 1. Comparative examples 1 and 2 were prepared in the same manner in a Ross mixer using the following procedure: 34g of silanol polymer was placed in a Ross mixer and 10g of plasticizer was placed in a Ross jar. Heating to 100 ℃. While mixing, slowly adding20g of Omya CaCO3. 2g of twice treated pyrogenic silica are also added. Mixing continued for 15 minutes. The dispersion was checked. An additional 15g of Omya CaCO was slowly added along with 2g of twice-treated fumed silica3And mixed for 30 minutes. The dispersion was again checked. An additional 15g of Omya CaCO was slowly added to the mixture, again with 2g of twice-treated fumed silica3And mixing was continued for 2 hours. The mixture was transferred to an airtight container.
And (3) curing operation: the mixture was then blended with catalyst, crosslinker and tackifier in the amounts and ingredients shown in tables 2 and 3, respectively, placed in a Hauschild flash mixer (Hauschild speedmixer) and held for 9-14 days for aging. The mixtures of comparative examples 1 and 2 were then removed and poured into a polytetrafluoroethylene mold having a depth of 1/4 ".
Comparative example 1 was prepared with the crosslinker methyltrimethoxysilane (MTMS) and the adhesion promoter tris (trimethoxysilylpropyl) isocyanurate (Iso-T) as shown in table 2:
TABLE 2
| Comparative example 1 | Silanol + CaCO3+ plasticizer + fumed silica | 48.5g |
| Catalyst and process for preparing same | Titanium isopropoxide ethyl acetylacetonate (Titanium isopropoxide ethyl acetylacetonate) | 0.5g |
| Crosslinking agent | MTMS | 0.9g |
| Tackifier | Iso-T | 0.2g |
Comparative example 2 was prepared as comparative example 1 except that the crosslinker Vinyltrimethoxysilane (VTMS) and adhesion promoter Iso-T were used as shown in table 3:
TABLE 3
| Comparative example 2 | Silanol + CaCO3+ plasticizer + fumed silica | 48.5g |
| Catalyst and process for preparing same | Titanium isopropoxide ethyl acetylacetonate | 0.5g |
| Crosslinking agent | VTMS | 0.9g |
| Tackifier | Iso-T | 0.2g |
Example 1 preparation of a sealing formulation:
TABLE 4
| Material | Amount in grams (g) |
| Silanol (30000cst) | 33 |
| OMYACARB FT-CaCO3 | 45 |
| ZnO | 5 |
| Secondary treated fumed silica | 6 |
| Dimethyl polysiloxane plasticizer | 10 |
Example 1 a sealing formulation was prepared using zinc oxide and the various ingredients shown in table 4. Example 1 a sealed formulation was prepared in a Ross mixer using the following procedure: 34g of silanol Polymer was placed in a Ross mixerAnd 10g of plasticizer was placed in a Ross jar. Heating to 100 ℃. While stirring, 15g of Omya CaCO was slowly added32g of twice-treated pyrogenic silica and 5g of zinc oxide. Mixing continued for 15 minutes. The dispersion was checked. An additional 15g of Omya CaCO was slowly added to the mixture3And 2g of twice-treated fumed silica. Mixing continued for 30 minutes. The dispersion was checked. An additional 15g of Omya CaCO was slowly added to the mixture3And 2g of twice-treated fumed silica. Mixing was continued for 2 hours. The mixture was transferred to an airtight container.
And (3) curing operation: the mixture was then blended with catalyst, crosslinker and tackifier in the amounts and ingredients shown in table 5 in a Hauschild flash mixer and held for 9-14 days for maturation. The mixture was then removed and poured into a teflon mold having a depth of 1/4 ".
Example 1 a sealant formulation was prepared with crosslinker MTMS and tackifier Iso-T:
TABLE 5
| Example 1 | Silanol + CaCO3+ plasticizer + fumed silica | 48.5g |
| Catalyst and process for preparing same | Titanium isopropoxide ethyl acetylacetonate | 0.5g |
| Crosslinking agent | MTMS | 0.9g |
| Tackifier | Iso-T | 0.2g |
Example 2 the ingredients of the sealing formulation are shown in table 6:
TABLE 6
| Material | Amount in grams (g) |
| Silanol (30000cst) | 34 |
| OMYACARB FT-CaCO3 | 40 |
| ZnO | 10 |
| Secondary treated fumed silica | 6 |
| Dimethyl polysiloxane plasticizer | 10 |
Example 2 a sealing formulation was prepared using zinc oxide and the various ingredients shown in table 6. Example 2 a sealed formulation was prepared in a Ross mixer using the following procedure: 34g of silanol polymer was placed in a Ross mixer and 10g of plasticizer was placed in a Ross jar. Heating to 100 ℃. While stirring, 15g of Omya CaCO was slowly added32g of twice-treated pyrogenic silica and 10g of zinc oxide. Mixing continued for 15 minutes. The dispersion was checked. Slowly add another 10g of Omya CaCO to the mixture3And 2g of twice-treated fumed silica. Mixing continued for 30 minutes. The dispersion was checked. An additional 15g of Omya CaCO was slowly added to the mixture3And 2g of twice-treated fumed silica. Mixing was continued for 2 hours. The mixture was transferred to an airtight container.
And (3) curing operation: the mixture was then blended with catalyst, crosslinker and tackifier in the amounts and ingredients shown in table 7 in a Hauschild flash mixer and held for 9-14 days for maturation. The mixture was then removed and poured into a teflon mold having a depth of 1/4 ".
Example 2 was prepared with crosslinker VTMS and tackifier Iso-T and the various ingredients in table 7:
TABLE 7
| Example 2 | Silanol + CaCO3+ plasticizer + fumed silica | 48.5g |
| Catalyst and process for preparing same | Isopropoxyethyl groupTitanium acetylacetonate | 0.5g |
| Crosslinking agent | VTMS | 0.9g |
| Tackifier | Iso-T | 0.2g |
Measurement of tack-free time and deep-section cure: after the formulations of examples 1-2 and comparative examples 1-2 were applied to polytetrafluoroethylene molds having a thickness of 1/4 ″, the surfaces were flattened with aluminum spacers (aluminum spacers). From the first application of the material, the surface was inspected at 15 minute intervals (minimum) with a 10g weight to determine whether the material was tack free until tack free. The tack free time data for examples 1-2 and comparative examples 1-2 are given in figure 3.
Deep-section cure was determined by the following solvent swell test: a portion of the resin according to examples 1-2 and comparative examples 1-2 weighed (about 5g samples were obtained from each of examples 1-2 and comparative examples 1-2) was obtained by cutting along the thickness of the mold and allowed to swell in 100ml of toluene for 3 days. The samples of examples 1-2 and comparative examples 1-2 were removed from the toluene and dried at ambient conditions for 3 days. Each sample was weighed again after drying. The weight difference provides the amount of uncured sample of examples 1-2 and comparative examples 1-2 dissolved in toluene. The measurements were taken at 6 hours, 24 hours, and 48 hours after the sealant examples were applied to the polytetrafluoroethylene mold. The percentages for the uncured examples are plotted against time.
The deep-section cure data for comparative example 1 and example 1 are given in fig. 4, and the deep-section cure data for comparative example 2 and example 2 are given in fig. 5.
While the method of the invention has been described with reference to certain embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed as the best mode contemplated for carrying out the process of the invention, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (25)
1. A construction element having at least two components bonded together or otherwise maintained in a sealed relationship with one another with a silicone rubber composition obtained by curing of a mixture comprising:
a) at least one silanol-terminated diorganopolysiloxane having the formula:
MaDbD′c
wherein a is 2, b is equal to or greater than 1, c is zero or a positive integer;
M=(HO)3-x-yR1 xR2 ySiO1/2;
wherein x is 0, 1 or 2, y is 0 or 1, provided that x + y is less than or equal to 2, R1And R2Is monovalent C1To C60A hydrocarbon group of (a);
D=R3R4SiO2/2;
wherein R is3And R4Is monovalent C1To C60A hydrocarbon group of (a); and
D′=R5R6SiO2/2;
wherein R is5And R6Independently selected from monovalent C1To C60A hydrocarbon group of (a);
b) at least one crosslinker for the one or more silanol terminated diorganopolysiloxanes;
c) at least one catalyst for the crosslinking reaction;
d) a deep-section fast-curing amount of zinc oxide having an average particle size of 50 to 70 nm; and
e) optionally at least one additional component selected from: alkyl-terminated diorganopolysiloxane, filler, ultraviolet stabilizer, antioxidant, tackifier, curing accelerator, thixotropic agent, plasticizer, moisture trapping agent, pigment, dye, surfactant, solvent, and antimicrobial agent.
2. The building element of claim 1, wherein the cross-linking agent, component (b), has the following general formula:
(R7O)(R8O)(R9O)(R10O)Si
wherein R is7、R8、R9And R10Independently selected from monovalent C1To C60A hydrocarbon group of (1).
3. The building element of claim 1, wherein the crosslinking agent, component (b), is at least one crosslinking agent selected from the group consisting of tetra-n-propyl silicate, tetraethyl orthosilicate, and methyltrimethoxysilane.
4. The architectural element of claim 1 wherein the catalyst, component (c), is a tin catalyst.
5. The architectural element of claim 4 wherein the tin catalyst is at least one catalyst selected from the group consisting of: dibutyltin dilaurate, dibutyltin diacetate, dibutyltin dimethoxide, tin octoate, isobutyltin tricarbonate, dibutyltin oxide, solubilized dibutyltin oxide, dibutyltin bis (diisooctylphthalate), dioctyltin bis (tripropoxysilyl), dibutyltin bis (acetylacetonate), dibutyltin silylate dioxide, methoxycarbonylphenyltin tris (suberate), isobutyltin tricarbonate, dimethyltin dibutyrate, dimethyltin dineodecanoate, triethyltin tartrate, dibutyltin dibenzoate, tin oleate, tin naphthenate, butyltin tris (2-ethylhexylhexanoate), tin butyrate and diorganotin bis (β -diketonate).
6. The building element of claim 1, wherein the catalyst, component (c), is a titanium compound.
7. The construction element according to claim 6, wherein said titanium compound is at least one compound selected from the group consisting of: di (isopropoxy) bis (ethylacetoacetate) titanium, di (isobutoxy) bis (ethylacetoacetate) titanium, di (n-butoxy) bis (ethylacetoacetate) titanium, bis (ethylacetoacetate) 1, 3-propylenedioxytitanium, isopropoxy (triethanolamine) titanium, di (methyl diglycolate) bis (triethanolamino) titanium, diisopropoxy (bis-2, 4-pentanedionate) titanium, ethoxyisopropoxy bis (2, 4-pentanedionate) titanium, bis (2, 4-pentanedionate) (2-EHA) titanium, tetra-n-butyl titanate, and tetra-isopropyl titanate.
8. The architectural element of claim 7 wherein the titanium compound is titanium bis (isopropoxy) bis (ethylacetoacetate).
9. The architectural element of claim 1 wherein the adhesion promoter is selected from the group consisting of: n-2-aminoethyl-3-aminopropyltrimethoxysilane, 1, 3, 5-tris (trimethoxysilylpropyl) isocyanurate, gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, bis- (gamma-trimethoxysilylpropyl) amine, N-phenyl-gamma-aminopropyltrimethoxysilane, triamino-functionalized trimethoxysilane, gamma-aminopropylmethyldiethoxysilane, methacryloxypropyltrimethoxysilane, methylaminopropyltrimethoxysilane, gamma-glycidoxypropylethyldimethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-glycidoxyethyltrimethoxysilane, beta- (3, 4-epoxycyclohexyl) propyltrimethoxysilane, beta- (3, 4-epoxycyclohexyl) ethylmethyldimethoxysilane, isocyanatopropyltriethoxysilane, isocyanatopropylmethyldimethoxysilane, beta-cyanoethyltrimethoxysilane, gamma-acryloxypropyltrimethoxysilane, gamma-methacryloxypropylmethyldimethoxysilane, 4-amino-3, 3, -dimethylbutyltrimethoxysilane, N-ethyl-3-trimethoxysilyl-2-methylpropylamine, and mixtures thereof.
10. The building element of claim 1, wherein the optional filler is selected from the group consisting of: clays, nanoclays, organoclays, ground calcium carbonate, precipitated calcium carbonate, colloidal calcium carbonate, calcium carbonate treated with compounds stearate or stearic acid; fumed silica, precipitated silica, silica gel, hydrophobized silica, hydrophilic silica gel, crushed quartz, ground quartz, alumina, aluminum hydroxide, titanium hydroxide, clay, kaolin, bentonite, montmorillonite, diatomaceous earth, iron oxide, carbon black and graphite, talc, mica, and mixtures thereof.
11. The architectural element of claim 1 wherein the nonionic surfactant is selected from the group consisting of: polyethylene glycol, polypropylene glycol, ethoxylated castor oil, oleic acid ethoxylate, alkylphenol ethoxylate, copolymer of ethylene oxide and propylene oxide, copolymer of silicone and polyether, copolymer of ethylene oxide and propylene oxide, copolymer of silicone, and mixtures thereof, the amount of the nonionic surfactant is 0.1 wt% to 10 wt%.
12. The architectural element of claim 1 wherein the amount of diorganopolysiloxane polymer, component (a), ranges in amount from 5 weight percent to 95 weight percent of the total composition.
13. The architectural element of claim 1 wherein the amount of diorganopolysiloxane polymer, component (a), ranges from 20 weight percent to 85 weight percent of the total composition.
14. The architectural element of claim 1 wherein the amount of diorganopolysiloxane polymer, component (a), ranges from 30 weight percent to 60 weight percent of the total composition.
15. The architectural element of claim 1 wherein the amount of the cross-linking agent, component (b), ranges from 0.1 to 10 weight percent of the total composition.
16. The architectural element of claim 1 wherein the amount of the cross-linking agent, component (b), ranges from 0.3 to 5 weight percent of the total composition.
17. The architectural element of claim 1 wherein the amount of the cross-linking agent, component (b), ranges in amount from 0.5 to 1.5 weight percent of the total composition.
18. The architectural element of claim 1 wherein the amount of catalyst, component (c), ranges in amount from 0.005 weight percent to 1 weight percent of the total composition.
19. The architectural element of claim 1 wherein the amount of catalyst, component (c), ranges in amount from 0.003 weight percent to 0.5 weight percent of the total composition.
20. The architectural element of claim 1 wherein the amount of catalyst, component (c), ranges in amount from 0.005 weight percent to 0.2 weight percent of the total composition.
21. The architectural element of claim 1 wherein the amount of zinc oxide, component (d), ranges in amount from 1 to 60 weight percent of the total composition.
22. The architectural element of claim 1 wherein the amount of zinc oxide, component (d), ranges from 2 to 30 weight percent of the total composition.
23. The architectural element of claim 1 wherein the amount of zinc oxide, component (d), ranges in amount from 5 to 20 weight percent of the total composition.
24. The architectural element of claim 1 wherein the amount of filler is from 0 to 90 weight percent of the total composition.
25. The architectural element of claim 1 wherein the tackifier is present in an amount of 0.5 to 20 weight percent of the total composition.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US11/728,899 | 2007-03-27 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| HK1142351A HK1142351A (en) | 2010-12-03 |
| HK1142351B true HK1142351B (en) | 2014-02-28 |
Family
ID=
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA2682191C (en) | Rapid deep-section cure silicone compositions | |
| US7993754B2 (en) | Architectural unit possessing rapid deep-section cure silicone rubber component | |
| JP5175266B2 (en) | Building unit with translucent silicone rubber component | |
| EP1723201B1 (en) | Rtv silicone composition offering rapid bond strength | |
| HK1142351B (en) | Architectural unit possessing rapid deep-section cure silicone rubber component | |
| HK1142351A (en) | Architectural unit possessing rapid deep-section cure silicone rubber component | |
| HK1142350A (en) | Rapid deep-section cure silicone compositions |