ES2274807T3

Insulating glass unit with structural primary sealant system

Abstract

An insulating glass unit (40), including: a first sheet (44) of glass; a second sheet (50) of glass; and a spacer system (56) including (i) a spacer (58) positioned between an inner surface (46) of the first glass sheet (44) and an inner surface (52) of the second glass sheet (50), and (ii) a sealing system (60) for adhering the inner surfaces (46, 52) of the sheets (44, 50) to the spacer (58), the sealing system (60) being a double seal system having two regions separate or distinct sealants (80, 82), including: at least one primary sealant (82), including: (a) at least one hot melt thermoplastic material having a melting temperature of the order of 125 ° F (51 ° C) to 250 ° F (121 ° C); and (b) at least one curable material, where the primary sealant, when cured, forms a covalent bond between the spacer (58) and the sheets (44, 50), and where the primary sealant has an initial hardness of the order of 25 Shore A to 45 Shore A and a post-cure hardness of the order of 30 Shore A to 65 Shore A and, when curing, a wet vapor transmission rate of less than 2.5 g / m2 / day, and a value of curing module on the order of 35 psi (2.5 kg / cm2) at 100 psi (7 kg / cm2), and a secondary sealant (80) that has a cured module higher than the primary sealant (82).

ES2274807T3, drawing sheet 1 — Sheet 1 of 1

Term

Term ended

Projected expiry passed 1 September 2020, 6.1 years ago.

19 claims: 1 independent, 18 dependent

1
ES 2 274 807 T3 REIVINDICACIONES 1. Una unidad de vidrio aislante (40), incluyendo:una primera hoja (44) de vidrio;una segunda hoja (50) de vidrio;y un sistema espaciador (56) incluyendo (i) un espaciador (58) colocado entre una superficie interior (46) de la primera hoja (44) de vidrio y una superficie interior (52) de la segunda hoja (50) de vidrio, y (ii) un sistema sellante (60) para adherir las superficies interiores (46, 52) de las hojas (44, 50) al espaciador (58), siendo el sistema sellante (60) un sistema de doble sello que tiene dos regiones sellantes separadas o distintas (80, 82), incluyendo: al menos un sellante primario (82), incluyendo: (a) al menos un material termoplástico de fusión en caliente que tiene una temperatura de fusión del orden de 125°F (51°C) a 250°F (121°C);y (b) al menos un material curable, donde el sellante primario, cuando está curado, forma un enlace covalente entre el espaciador (58) y las hojas (44, 50), y donde el sellante primario tiene una dureza inicial del orden de 25 Shore A a 45 Shore A y una dureza post-curación del orden de 30 Shore A a 65 Shore A y, al curar, una tasa de transmisión de vapor húmedo inferior a 2,5 g/m 2 /día, y un valor de módulo curado del orden de 35 psi (2,5 kg/cm 2 ) a 100 psi (7 kg/cm 2 ), y un sellante secundario (80) que tiene un módulo curado más alto que el sellante primario (82).
2
La unidad de vidrio aislante (40) según la reivindicación 1, donde el material termoplástico de fusión en caliente incluye de 10% a 90% en peso del sellante primario.
3
La unidad de vidrio aislante (40) según la reivindicación 1, donde el material termoplástico de fusión en caliente y el material curable son los mismos, incluyendo especialmente cada uno un material seleccionado de prepolímeros de uretano conteniendo silicio de peso molecular alto y copolímeros de acrilonitrilo butadieno conteniendo silicio.
4
La unidad de vidrio aislante (40) según la reivindicación 1, donde el material termoplástico de fusión en caliente incluye al menos un material seleccionado de poliolefinas, acetatos de polivinilo, poliamidas, hidrocarbonos, asfaltos, bitúmenes, ceras, parafinas, cauchos crudos, cauchos fluorados, cloruros de polivinilo, poliamidas, fluorocarbonos, poliestirenos, resinas celulósicas, acrílicos, elastómeros termoplásticos, polímeros de estireno butadieno, politerpenos, terpolímeros de etileno-propileno, y sus mezclas.
5
La unidad de vidrio aislante (40) según la reivindicación 1, donde el material termoplástico de fusión en caliente incluye un material seleccionado de parafina clorada sólida, poliisobutileno, aceite de soja epoxidizado, butilacrilato de etileno, poliolefina, y sus mezclas.
6
La unidad de vidrio aislante (40) según la reivindicación 1, donde el material termoplástico de fusión en caliente incluye una mezcla de un material epoxídico, un material de acrilato, y un material de poliolefina.
7
La unidad de vidrio aislante (40) según la reivindicación 1, donde el material curable incluye de 5% a 50% en peso del sellante primario.
8
La unidad de vidrio aislante (40) según la reivindicación 1, donde el material curable polimeriza a la exposición a un constituyente de la atmósfera, incluyendo especialmente el constituyente un material seleccionado de oxígeno, vapor de agua, y sus mezclas.
9
La unidad de vidrio aislante (40) según la reivindicación 1, donde el material curable incluye un material seleccionado de materiales curables por UV, materiales curables por IR, materiales curables por humedad, materiales curables por oxígeno, materiales curables por temperatura, y sus mezclas.
10
La unidad de vidrio aislante (40) según la reivindicación 1, donde el material curable incluye un material seleccionado de poliuretanos alcoxi silano terminados, poliéteres alcoxi silano terminados, resinas de polidimetilsiloxano, silanos organo funcionales, y sus mezclas.
11
La unidad de vidrio aislante (40) según la reivindicación 1, incluyendo además un aditivo seleccionado de plastificantes, rellenos, pigmentos, catalizadores, aceleradores, mejoradores de resistencia a la intemperie, y sus mezclas. ES 2 274 807 T3
12
La unidad de vidrio aislante (40) según la reivindicación 1, donde el sellante primario es un primer sellante y la unidad incluye además un segundo sellante situado junto al primer sellante.
13
La unidad de vidrio aislante (40) según la reivindicación 12, donde el segundo sellante es un sellante termoestable.
14
La unidad de vidrio aislante (40) según la reivindicación 12, donde el segundo sellante se selecciona de sellantes de silicona, polisulfuro, y poliuretano.
15
La unidad de vidrio aislante (40) según la reivindicación 1, donde el sellante secundario (80) tiene un módulo curado superior a 75 psi (5,3 kg/cm 2 ).
16
La unidad de vidrio aislante (40) según la reivindicación 1, donde al menos una de las hojas tiene un recubrimiento dispuesto encima.
17
La unidad de vidrio aislante (40) según la reivindicación 6, donde el material termoplástico o material termoplástico de fusión en caliente incluye una mezcla de plastificante de soja epoxidizado, butilacrilato de etileno, y una poliolefina, especialmente poliolefina amorfa.
18
La unidad de vidrio aislante (40) según la reivindicación 1, donde el sellante primario incluye un acelerador incluyendo especialmente un material de amina bloqueado.
19
La unidad de vidrio aislante (40) según la reivindicación 1, donde el sellante primario incluye un agente de pegajosidad incluyendo especialmente un éster de rosina de madera o ésteres de rosina de madera seleccionados, resinas de hidrocarbono, resinas terpeno fenólicas, y resinas alfa metil estireno.

Independent claims19

312 paragraphs in 16 sections, as filed

ES 2 274 807 T3

DESCRIPTION

Insulating glass unit with a structural primary sealant system.

1. Field of the invention

This application relates generally to insulating glass units and more particularly to an insulating glass unit having a double seal system that provides good protection against moisture vapor permeability as well as better structural integrity.

2. Technical considerations

Insulating glass (IG) units are used in a wide variety of applications, such as skylights, high temperature environmental viewing windows, and architectural windows, to name just a few. IG units are typically used to reduce heat transfer, such as between the interior and exterior of a building.

A typical IG unit is made up of two panes of glass separated near their edges by a spacer to provide a chamber between the two panes of glass. This chamber is typically filled with a selected insulating atmosphere, such as argon, to improve the insulating characteristics of the IG unit. A sealing system is used to bond the two panes of glass to the spacer. The sealing system is expected to provide sufficient structural strength to maintain the unit of the IG unit and also to provide sufficient protection against the escape of the insulating atmosphere from the chamber and / or entry into the humid vapor chamber from the ambient atmosphere outside. of the IG unit. Examples of conventional IG units are described in US Patent Nos. 4,193,236, 4,464,874, 5,088,258, and 5,106,663; and the European reference EP 65510.

The strength and performance of the IG unit are strongly dependent on the sealant system and the type of sealant used to fix the glass sheets to the spacer. Most sealants currently in use can be broadly divided into two main types: (1) "structural sealants" and (2) "low moisture vapor transmission (MVT) sealants".

Structural sealants form a covalent chemical bond between the glass sheet and the spacer and promote the structural integrity of the IG unit. Examples of structural sealants include thermosetting materials, such as polysulfides, polyurethanes, and silicone. These thermosets typically have a relatively high "modulus". As those of ordinary skill in the art of IG units will understand, the term "modulus" refers to the stress / strain ratio of a material, that is, the force required to stretch or elongate a material a certain distance. Modulus is conventionally defined as the slope of the stress / strain curve for a material and can be calculated according to ASTM D412. The higher the modulus value, the more force is required to elongate or stretch the material, that is, the stronger the material. Thermosetting polyurethane, polysulfide, and silicone materials typically have modulus values in the range of several hundred psi. Improving the structural integrity of the IG unit, structural sealants typically provide poor MVT characteristics, for example 10 g / m2/ day or more (measured per ASTM F1249), and also provide relatively high gas transmission rates. For example, polyurethane, polysulfide, and silicone materials typically have MVT rates in the range of about 15, 25, and 50 g / m2.2/ day, respectively. As a result, IG units made only with conventional structural sealants do not typically provide commercially acceptable MVT characteristics or gas retention properties.

On the other hand, low MVT sealants, which do not covalently bond to the glass sheets and / or the spacer, provide better mVt characteristics, for example less than 10 g / m2/ day, and better gas barrier capabilities compared to structural sealants, but provide poorer structural integrity. Examples of low MVT sealants include thermoplastic materials, such as hot melt materials, eg, polyisobutylene (PIB). PIB materials typically have an MVT value of about 1.0 g / m2/ day or less.

Additionally, thermoplastic hot melt sealants typically must be applied at temperatures above 300 ° F (149 ° C). This high temperature requirement can lead to higher manufacturing costs due to higher power consumption and the need for specialized high temperature equipment. Furthermore, these thermoplastic materials typically have a lower modulus than thermoset materials, that is, thermoplastic materials require less force to stretch or elongate and have a tendency to cold flow. For example, PIB has a modulus value of approximately 30 psi (2.1 kg / cm2). Therefore, thermoplastic sealants are subject to softening when exposed to heat and, when placed under load, can excessively flow or deform releasing the load. As a result, IG units made only with conventional thermoplastic sealants do not typically provide commercially acceptable structural characteristics.

A problem with using a single sealant for an IG unit having a conventional rigid spacer arises from differences in sealant thickness in the sealant system. For example, the thickness (width) of the sealant between

ES 2 274 807 T3 the side of the spacer and the adjacent glass sheet (side region) is much less than the thickness of the sealant located between the glass sheets outside the spacer (outer region). Therefore, if one of the glass sheets is displaced out of the spacer, for example due to a change in atmospheric pressure, the relative elongation percentage for the thinner sealing portion in the side region is much greater than for the thickest sealing portion in the outer region. This means that the thinner sealing portion in the side region bears practically the entire load of the sealing system, which can cause this sealing portion to crack or fail prematurely.

Recently, attempts have been made to develop "hybrid" sealants for single IG sealant units that have the low MVT characteristics of a thermoplastic material with the structural characteristics of a thermoset material. For example, US Patent No. 5,849,832 describes a single component sealant that combines a hot melt thermoplastic resin mixed with an atmospheric cure polymer. The MVT characteristics of this sealant, for example about 3.0-4.0 g / m2/ day, they are better than the MVT characteristics of conventional thermoset sealants, but still higher than thermoplastic sealants, such as PIB. Additionally, since this sealant provides structural integrity to the IG unit, it has a modulus of approximately 250 psi (17.5 kg / cm2). In addition, this material is harder than conventional thermoplastic materials, for example, it has an initial hardness greater than about 50 Shore A and a cured hardness greater than about 60 Shore A (measured according to test procedure P.1.A of the Sealed Insulating Glass Unit Manufacturers Association (SIGMA) Using a Shore gauge (A scale) commercially available from the Shore Instrument Company). Therefore, this material does not completely overcome the drawbacks explained above.

As an alternative to single sealant systems, so-called “double seal” systems were developed to combine the relative advantages of structural sealants and low MVT sealants. A conventional double seal system utilizes an inner or primary low MTV thermoplastic sealant located primarily in the spacer side region to reduce the transmission of wet vapor to the chamber. This primary sealant provides little or no structural integrity to the IG unit. A secondary exterior structural thermoset sealant is located primarily on the exterior of the spacer (outer region) to bond the spacer and panes of glass to provide structural integrity to the IG unit.

However, even in these double seal systems, in normal use there is a natural tendency for the outer edges of the glass sheets to twist or flex due to changes in atmospheric pressure, temperature, wind load, or altitude changes. Under these circumstances, the primary thermoplastic sealant tends to expand and contract and may separate from the glass sheet and / or the spacer. This can cause gaps in the sealing system through which moisture can enter the chamber or through which the insulating atmosphere can escape the chamber.

Therefore, it would be advantageous to provide a double seal system for an IG unit that provides low MVT characteristics, but also provides better structural performance over conventional sealing systems. It would also be desirable for the primary sealant of the sealant system to possess a lower modulus value than conventional structural sealants or hybrid sealants to reduce the stress typically borne by primary sealants located in the side region of an IG unit.

Summary of the invention

An insulating glass unit of the invention includes a first sheet of glass, a second sheet of glass, and a spacer system. The spacer system includes (i) a spacer positioned between an inner surface of the first glass sheet and an inner surface of the second glass sheet and (ii) a sealant system for adhering the inner surfaces of the glass sheets to the spacer. The sealant system is a double seal system having two separate or distinct sealing regions including a primary sealant including (a) at least one hot melt thermoplastic material having a melting temperature on the order of 125 ° F (52 ° C). ) at 250 ° F (121 ° C), and (b) at least one curable material. The sealant, when cured, forms a covalent bond between the spacer and the sheets. The sealant has an initial hardness of the order of 25 Shore A to 45 Shore A and a post cure hardness of between 30 Shore A and 65 Shore A and, upon curing, a wet vapor transmission rate of less than 2.5 g / m2/ day, and a cured modulus value of 35 psi (2.5 kg / cm2) 35 psi (2.5 kg / cm2) at 100 psi (7 kg / cm2).

Another insulating glass unit includes a first sheet having an inner surface and an outer surface and a second sheet having an inner surface and an outer surface, with the sheets positioned such that the inner surface of the first sheet faces the inner surface of the second sheet. A spacer is located between the first and second sheets and a sealing system adheres the sheets to the spacer. The sealant system includes (a) the first or primary sealant including a thermoplastic material and a curable material, and (b) a secondary sealant. The primary sealant has a wet vapor transmission rate of less than 2.5 g / m2/ day and a hardness after curing of the order of 30 Shore A to 65 Shore A and a cured modulus less than the secondary sealant to reduce the deformation in the primary sealant produced when the IG unit flexes, the cured modulus value being the primary sealant on the order of 35 psi (2.5 kg / cm2) at 100 psi (7 kg / cm2).

ES 2 274 807 T3

Brief description of the drawing

The above summary, as well as the following detailed description of the preferred embodiments, will be better understood when read in conjunction with the accompanying drawing, in which:

Figure 1 is a cross section of an elevational view of a portion of a joint edge of an IG unit having a sealing system according to the invention.

Description of the preferred embodiments

As used herein, spatial or directional terms such as "inside", "outside", "left", "right", "rear" and the like refer to the invention as depicted in the drawing figure. However, it is to be understood that the invention can assume various alternative orientations and step sequences without departing from the novel concepts described herein. Accordingly, such terms are not to be considered limited, unless otherwise indicated. Furthermore, with the exception of operating examples, or where otherwise indicated, all numbers expressing amounts of ingredients, reaction conditions, etc., used in the specification and claims are to be understood as modified in all cases by the term "approximately". In addition, all numerical references to amounts, unless otherwise specified, are "by weight". In addition, all the ranges described here must be understood as covering each and every one of the subtrangas subsumed in them. For example, a range from "1 to 10" includes each and every one of the subranges between (and including) the minimum value of 1 and the maximum value of 10, that is, each and every one of the subranges that have a value minimum of equal to or greater than 1 and maximum value of equal to or less than 10, for example, 5.5 to 10.

An IG unit 40 according to the present invention is shown in Figure 1. The IG unit 40 has a first sheet 44 having an inner surface 46 and an outer surface 48. The first sheet 44 is spaced from a second sheet 50, which also it has an inner surface 52 and an outer surface 54. The two sheets 44 and 50 may be of any material conventionally used in the IG unit art. For example, although not to be considered limiting, the two sheets 44 and 50 can be made of clear glass, eg floating clear glass, or one or both sheets can be of colored glass. The glass can be annealed, tempered, or heat-strengthened glass and can be uncoated or coated glass.

The inner surface 46 of the first sheet 44 faces the inner surface 52 of the second sheet 50, and the inner surfaces 46 and 52 are spaced apart by a spacer system 56 having a spacer 58 attached, for example, with adhesive, to the two sheets 44 and 50 by a sealant system 60 having two sealants. Spacer 58 can be any of the types used in the IG unit art, such as a conventional rigid or box-type spacer, a U-shaped spacer, or a flexible spacer. Such spacers are typically formed of metal, such as aluminum or 201 or 304 stainless steel, and are bent or shaped to a conventional spacer shape. Examples of suitable spacers are described, for example, but not to be considered limiting, in U.S. Patent Nos. 4,193,236,4,464,874, 5,088,258, 5,655,282, 5,675,944, 5,177,916, 5,255 .481, 5,351,451, 5,501,013, and 5,761,946, which are incorporated herein by reference. In the illustrative embodiment depicted in FIG. 1, although it is not to be construed as limiting the invention, the spacer 58 is illustrated as a box-type spacer having a base 66 with a first side 72 and a second side 74 that intersect. extends from base 66. Each side 72, 74 includes an outer surface 76, 78 facing inner surfaces 46, 52 of respective adjacent sheets 44, 50.

The two sheets 44 and 50 and the spacer system 56 define a chamber 62 or "dead space" between the two sheets 44 and 50. The chamber 62 can be filled with an insulating atmosphere, such as air or argon or krypton gas. A conventional desiccant material 64 in the art may be placed within the spacer 58, for example, the desiccant material may be loose or may be adhesively bonded to one of the interior surfaces of the spacer 58 in a conventional manner. Spacer 58 preferably includes channels or holes 65 through which desiccant material 64 is in contact with insulating gas in chamber 62.

A coating 70, such as a solar control coating, eg, low-emissivity or photocatalytic, such as MSVD, CVD, pyrolysis, sol-gel, etc., can be applied in a conventional manner to a surface, eg, a surface. interior, single or multiple sheets 44 and 50.

The sealing system 60 of the present invention is a "double seal" system having two separate or distinct sealing regions, that is, an outer or secondary sealant 80 and an inner or primary sealant 82, using a sealing composition of the invention to form the primary sealant 82.

The primary sealant 82 is located primarily in the lateral regions of the spacer 58, that is, the majority of the sealant is located between one side of the spacer 58 and the adjacent sheet 44 or 50. However, unlike conventional primary sealants that provide low MVT characteristics, but little or no structural integrity, the primary sealant 82 of the invention is covalently bonded to sheets 44 and 50 and spacer 58 to provide IG 40 unit not only good structural integrity, but also to provide a low moisture vapor transmission rate that is generally comparable to conventional primary thermoplastic sealants, as GDP.

ES 2 274 807 T3

Preferably, the primary sealant 82 has a wet vapor transmission rate of less than 10 g / m2/ day, preferably less than 5 g / m2/ day, more preferably less than 3 g / m2/ day, and most preferably less than 2 g / m2/day.

Primary sealant 82 preferably has a lower cured modulus value than secondary sealant 80 to reduce deformation in primary sealant 82 produced when IG unit 40 flexes. Preferably, the primary sealant 82 has a cured modulus value of less than 200 psi (14 kg / cm2), preferably less than 150 psi (10.5 kg / cm2), and more preferably 35 psi (2.5 kg / cm2) at 120 psi (8.4 kg / cm2).

As will be more specifically described in the following examples, the primary sealant 82 of the present invention is formed of a sealant composition including a hot melt thermoplastic material and a curable material.

The hot melt material can include a single hot melt material or it can be a mixture of several chemically different hot melt materials. The hot melt material can include one or more polyolefins, such as polyethylenes, or can include polyvinyl acetates, polyamides, hydrocarbon resins, asphalts, bitumens, waxes, paraffins, crude rubbers, fluorinated rubbers, polyvinyl chloride, polyamides, fluorocarbons, polystyrene, polypropylenes, cellulosic resins, acrylic resins, thermoplastic elastomers, styrene butadiene resins, ethylene propylene terpolymers prepared from ethylene propylene diene monomer, polyterpenes, and mixtures thereof. For example, in an exemplary embodiment, the hot melt thermoplastic material can include a mixture of solid chlorinated paraffin and an epoxidized soybean oil. In an exemplary alternative embodiment, the hot melt material may include a mixture of solid chlorinated paraffin and polyisobutylene. In a presently preferred embodiment, the hot melt material includes a blend of an epoxidized soy plasticizer, ethylene butylacrylate (EBA), and a polyolefin material.

Preferably, the hot melt thermoplastic material of the primary sealant composition is present in an amount from 10% by weight to 90% by weight, more preferably 20% by weight to 70% by weight, even more preferably 25% by weight at 65% by weight, and most preferably 25% by weight to 35% by weight, based on the total weight of the primary sealant composition.

The primary sealant includes at least one curable material, which curable material may be a radiant energy curable material, such as an IR or UV curable material, a heat curable material, or an atmospheric curable material, such as a polymeric material that it crosslinks upon exposure to a constituent of the ambient atmosphere, such as oxygen or water vapor. The curable material may include one or more moisture-curable polysulfides, polydimethylsiloxanes, oxygen-curable polysulfides, and mixtures thereof, which may contain silicon functionalities. Curable materials suitable for the practice of the invention include alkoxy, acetoxy, oxyamino silane terminated polyethers and polyether urethanes; alkyl solxane polymers crosslinked with organo functional alkoxy, acetoxy, oxyamino silanes; moisture curable isocyanate functional polyoxyalkalene polymers and polyalkalene polymers; thiol functional polymers and oligomers (such as polyethers, polyether urethanes, polysulfides, polythioethers), suitably catalyzed to produce moisture curable systems; epoxy functional polymers and oligomers with moisture unblockable crosslinkers; Functional acrylic polymers with unblockable cross-linkers, UV-curable acrylic polymers, and blends thereof. Most preferably, the curable material includes one or more alkoxy silane terminated polyurethanes, alkoxy silane terminated polyethers, polydimethylsiloxane polymers, organo functional silanes, and mixtures thereof. In a currently preferred embodiment, the curable material includes one or more moisture curable polyurethanes, such as PERMAPOL MS.® polyurethane, commercially available from PRC Desoto of Glendale, California.

The curable material of the primary sealant composition is preferably present in the composition in an amount of 5% by weight to 50% by weight, preferably 10% by weight to 40% by weight, more preferably 10% by weight to 28% by weight , and most preferably 10% by weight to 15% by weight, based on the total weight of the sealant composition.

Furthermore, in a presently preferred embodiment, the primary sealant composition also includes a tackifier, such as wood rosin ester, to provide adhesion upon initial application of the composition and before covalent bonding occurs. Examples of other suitable tackifiers include hydrocarbon resins, phenolic terpene resins, and alpha methyl styrene resins. The tackifier may be present in any suitable amount, for example, but is not to be considered limiting, 5% by weight to 50% by weight based on the total weight of the sealant composition.

As explained above, the primary sealant composition of the invention may further include a catalyst, such as an organic catalyst. The specific organic catalyst and the amount used will depend on the particular curable material that is used. Suitable catalysts include organotin compounds, aliphatic titanates (having 1-12 carbon atoms) such as lower alkyl titanates, and amines. Suitable catalysts include dibultyltin dilaurate, dibultyltin diacetate, tetrabutyl titanate, and tetraethyl titanate. Although the sealant composition of the invention will cure without the addition of the catalyst, the addition of a catalyst can allow for faster cure times, which can be advantageous in some situations.

ES 2 274 807 T3

Similarly, an accelerator can be added to further increase cure rates. The specific accelerator will be dictated by the identity and concentration of the catalyst and will be chosen from those common in the art. Examples of suitable accelerators include blocked amines, such as bis-oxazoladine, which is commercially available as "HARDNER OZ" from Bayer, Inc.

The sealant composition can include catalysts, accelerators, plasticizers, fillers, pigments, weatherability improvers, and similar components known in the art. It may also be desirable, in some cases, to add additional fillers, such as talc, calcium carbonate, silicas, and silicates, pigments, rheological agents, and the like as known in the art. The strength properties in the sealant depend on the type and amount of the hot melt material, and also on the selection of filler. Fillers can be selected by those skilled in the art and added in an amount sufficient to impart appropriate strength, as well as to impart desirable application properties to the sealant composition. The primary sealant composition of the present invention should be easy to handle and apply to the IG unit.

The hot melt thermoplastic material, the curable material, and any optional components are preferably combined to form a single primary sealant material. By "single material" it is meant that on a macroscopic scale the sealant includes a substantially homogeneous mixture; however, it can have compositional variations on a microscopic scale.

In an alternative embodiment, the hot melt thermoplastic material and the curable material can be the same. A preferred formulation includes high molecular weight silicon-terminated urethane prepolymers. Another formulation includes silicon-functionalized Kraton polymers (block copolymers, commercially available from Shell Chemical Company). Kraton polymers are block copolymers of various types such as SBS (styrene-butadiene-styrene), SIS (styrene-isoprene-styrene), and SEBS (styrene-ethylene / butylene-styrene). Another formulation includes Kraton polymers with other functional groups that undergo rapid solidification on cooling, followed by chemical cure on exposure to atmospheric conditions.

The secondary sealant 80 is preferably a conventional structural sealant, such as a conventional thermoset sealant material. For example, secondary sealant 80 may include one or more conventional silicone, polyurethane, or polysulfide structural sealant materials known in the art. Examples of suitable secondary sealant materials are described, for example, in US Patent Nos. 4,193,236, 4,464,874, 5,088,258, and 5,106,663, and European reference EP 65510. Alternatively, sealant PRC 590, commercially available from PRC Desoto International, Inc., of Glendale, California, can be used as the secondary sealant 80. US Patent No. 5,849,832, incorporated herein by reference, also describes a suitable material as a secondary sealant for the present invention. In a presently preferred embodiment, the secondary sealant 80 is a conventional silicone sealant material. As will be understood by those of ordinary skill in the art, the primary function of the secondary sealant 80 is to provide structural integrity to the IG 40 unit. Therefore, the secondary sealant preferably has a modulus value greater than 75 psi (5.3 kg / cm2), preferably greater than 125 psi (8.8 kg / cm2), and more preferably greater than 200 psi (14 kg / cm2) measured according to ASTM D412. As depicted in Figure 1, the secondary sealant 80 preferably extends across the width of the exterior of the spacer 58 (outer region), for example, it extends through the perimeter groove formed by the outer surface of the base 66. of the spacer 58 and the outer marginal edges of the blades 44 and 50.

The sealants 80, 82 can be of any suitable dimensions to adhere the sheets 44, 50 to the spacer 58. For example, the primary sealant 82 can have a thickness of 3/32 inch (0.2 cm) to 3/16 inch ( 0.5 cm) and the secondary sealant 80 can be 3/16 inch (0.5 cm) to 1/4 inch (0.6 cm) thick.

The method of manufacturing an IG unit 40 incorporating a sealing system 60 of the invention will now be described. As will be appreciated, the IG unit 40 and spacer 58 can be manufactured in a conventional manner, such as, but not limited to, those described in U.S. Patent Nos. 4,807,439, 4,831,799, 4,431,691, 4,873,803 , and 3,919,023, but modified as explained below to include the sealing system 60 of the invention. For example, a substrate, such as a metal foil of sufficient thickness, length, and width to produce a spacer of desired dimensions, can be formed by conventional rolling, bending, or shaping techniques. Although the primary and secondary sealants 82, 80 can be placed on the substrate prior to forming, it is preferred to apply the primary and secondary sealants 82, 80 after the spacer 58 has been formed. The primary and secondary sealants 82, 80 can be applied in any order on the spacer 58. However, it is preferred to apply the primary sealant 82 first and then the secondary sealant 80. For example, the primary sealant 82 can be applied to the sides. 76,78 of the spacer 58 by a set of nozzles and the secondary sealant 80 can subsequently be applied to the rear or base 66 of the spacer 58 by a separate set of nozzles. Sealants 80, 82 can be applied in any desired thickness.

The IG unit 40 can then be assembled by positioning and adhering the sheets 44 and 50 to the spacer 58 by the sealing system 60. An insulating gas, such as air or argon or krypton gas, can be introduced into the chamber 62 in a conventional manner.

The primary sealant 82 is preferably flowable or, more preferably, is a high viscosity liquid, for example, having a viscosity of about 50,000 poise, at a temperature greater than 160 ° F (71 ° C) to 170 ° F.

ES 2 274 807 T3 (77 ° C). The primary sealant 82 of the invention is preferably applied at an elevated temperature of about 125 ° F (51 ° C) to 250 ° F (121 ° C) as a high-viscosity liquid or paste, which is then solidified. when cooled to a temperature of 90 ° F (32 ° C) to 100 ° F (38 ° C). The hot melt material of the sealant functions as the meltable component during initial application and provides strength on cooling. The curable material then begins to cure, for example, by reaction with atmospheric moisture or heat, forming a cross-linked elastomer that resists deformation upon application of heat. After the curable material has cured, the hot melt material functions as a plasticizer within the cured polymer phase.

The primary sealant 82 of the invention has an initial pre-cure hardness of between 25 Shore A and 45 Shore A. The cured primary sealant 82 has a hardness of between 30 Shore A and 65 Shore A, preferably a hardness at about 48 hours after application between 30 Shore A and 50 Shore A or more.

A method of making the primary sealant of the invention will now be explained. The primary sealant 82 of the present invention can be prepared in the following general manner, with more specific preparations being described in the following examples. The hot melt thermoplastic material, or mixtures thereof, is first dispensed into a mixing vessel at elevated temperature. In a preferred embodiment, the mixing vessel is a stainless steel vessel capable of mixing under a vacuum of 20 Torr or less and further includes a mixer having a variable speed, multi-axis unit, with a low speed sweeping blade. , a high speed spreader, and a low speed auger. The filler material is subsequently added to the hot melt material and mixing begins at low speed. Next, the curable material, or mixtures thereof, to which additional filler can be added to form a curable composition, is added to the mixture after spinning under vacuum. At the point where the curable material is preferably added, mixing is performed under vacuum in order to eliminate or reduce the exposure of the mixture to atmospheric conditions, and also to remove residual water from the raw materials, thereby improving the package stability. Additives can be added in a small volume such as pigments, weatherability improvers such as UV absorbers and antioxidants and the like before the introduction of the curable material, while any catalyst can be added afterwards. The material is kept in substantially dry conditions until it is ready to be applied to the IG unit. In other preferred embodiments, mixing can be carried out under a blanket of dry inert gas. Specific non-limiting exemplary methods of making the primary sealant of the invention are described in the following examples.

As explained above, any suitable structural sealant, such as a conventional silicone sealant material, can be used as the secondary sealant 80.

Example 1

This example illustrates, as set forth in Table 1, a suitable primary sealant composition of the invention and a method of making the primary sealant.

(Table goes to next page)

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Note: The stainless steel container was preheated to 180 ° F (82 ° C), maintaining this temperature throughout the process. The applied vacuum was less than or equal to about 20 Torr.

1 CERECHLOR S52, a long chain normal paraffin, 52% chlorine, commercially available from ICI, Inc.

2 PARAPLEX G-62, a high molecular weight soybean oil epoxide commercially available from Rohm and Haas.

3 CHLOREZ 700-S, a 70% chlorine long chain normal paraffin commercially available from Dover Chemical Company.

4 Commercially available from Columbia Carbon Company.

5 Commercially available from Specialty Metals Corporation.

6 As described in Table 2 below.

7 Commercially available from Air Products Corporation.

8 Bis-oxazoladine, commercially available as HARDNER OZ from Bayer, Inc.

TABLE 2

<td colspan="4">COMPOSITION OF ATMOSPHERIC CURING RESIN</td>

<td>MATERIAL</td><td>LOAD WEIGHT</td><td>% IN WEIGHT</td><td>PROCESS</td>

<td>1. PERMAPOL MS®1</td><td>950.0 lbs. (428 kg)</td><td>58.3 OR 0</td><td>Low speed loading and mixing</td>

<td>2. Organ silane functional Π2</td><td>13.5 lbs (6.0 kg)</td><td>0, 83 OR, or</td><td>Load</td>

<td>3. Organo functional silane # 23</td><td>13.5 lbs (6.0 kg)</td><td>0.83 0 or</td><td>Load</td>

<td>4. Talc</td><td>652.0 lbs. (293 kg)</td><td>40.0 or or</td><td>Loading a bag at once. Vacuum was activated (less than or equal to about 20 Torr). It was mixed evenly. The moisture content was checked.</td>

1 Commercially available from PRC Desoto International, Inc.

2 A-171 vinyltrimethoxysilane commercially available from OSI, Inc.

3 A-187 glycidoxypropyltrimethoxysilane commercially available from OSI, Inc.

ES 2 274 807 T3

Example 2

This example illustrates another suitable primary sealant composition of the invention and a method of making it.

CQ

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ES 2 274 807 T3

Example 3

This example illustrates a presently preferred primary sealant composition of the invention and the method of making it.

TABLE 4

<td>MATERIAL</td><td>% IN WEIGH</td><td>PROCESS</td>

<td>Epoxidized soy plasticizer</td><td> 6, 5</td><td>Load.</td>

<td>Drying oil1</td><td> 1,1</td><td>Load.</td>

<td>Modified phenolic drying oil2</td><td> 1,1</td><td>Carqa.</td>

<td>Polyolefin amorphous3</td><td> 11,6</td><td>Slow charge with mixer on, beginning heating at 210 ° F (99 ° C) with steam.</td>

<td>Ethylene Butyl Acrylate (EBA)4</td><td> 11, 6</td><td>Slow loading with mixer activated.</td>

<td>Wood rosin ester5</td><td> 28,1</td><td>Slow loading with mixer activated.</td>

<td>Titanium dioxide6</td><td> 2,1</td><td>Load. It was mixed until the material was fluid, subsequently turning off the steam.</td>

<td>talcum powder</td><td> 19, 5</td><td>Slow loading with mixer activated After half loading, vacuum was drawn in and mixed for 10 minutes. The mixer was opened and the rest of the material was loaded. Mix for 40 minutes under full vacuum.</td>

<td>Epoxidized soy plasticizer</td><td> 1</td><td>Used for pasta with the following three raw materials.</td>

<td>Organo- silane functional 37</td><td> 0, 5</td><td>Mix in the pasta with the previous raw material.</td>

<td>Dilaurate multi-tin</td><td> 0,07</td><td>Mix in the pasta with previous raw materials.</td>

<td>Throttle</td><td> 0, 17</td><td>Pasta with the previous raw materials, later loading into the batch with the mixer activated. He breathed in and closed the vacuum. It was mixed under vacuum for 15 minutes.</td>

<td>Intermediate Ayou</td><td> 16, 8</td><td>It was mixed with the above mixture in process equipment at 210 ° F (99 ° C) at 225 ° F (107 ° C)</td>

Note: The vacuum used was less than or equal to approximately 20 Torr.

1 Commercially available from Industrial Oil Company.

2 Commercially available from HP Polymer Company.

3 Commercially available from Huls Company.

4 Commercially available from Elf Atochem.

5 Commercially available from Arizona Chemical Company.

6 Commercially available from EI DuPont de Nemours and Company.

7 Mercaptopropyltrimethoxysilane commercially available from OSI.

8 As described in Table 5 below.

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TABLE 5

<td>INTERMEDIATE A</td><td></td><td></td>

<td>MATERIAL</td><td>% IN WEIGHT</td><td>PROCESS</td>

<td>PERMAPOL MS®</td><td> 10,3</td><td>Load.</td>

<td>talcum powder</td><td> 6,2</td><td>Loading with mixer activated.</td>

<td>Black from Coal</td><td> 0,034</td><td>Loading with mixer activated. Full vacuum and mix for one hour. Maximum temperature 150 ° F (66 ° C). Sample to laboratory to check water content.</td>

<td>Organofunctional silane 1</td><td> 0, 10</td><td>Loading with mixer activated.</td>

<td>Organofunctional silane 2</td><td> 0, 15</td><td>Loading with mixer activated. Aspiration and vacuum closing. Blend for 20 minutes.</td>

Note: The vacuum used was less than or equal to approximately 20 Torr.

Comparative Example 4

Tests were performed on primary sealant compositions formed according to Example 3 above, and Table 6 sets forth the test results (numerical mean) for tests using the primary sealant composition of the invention as a function of those of a polyisobutylene primary sealant material ( PIB) conventional commercially available from ADCO Products of Michigan City, Michigan.

TABLE 6

<td>MVT</td><td>GDP</td><td>PRIMARY SEALANT</td>

<td>Peeled (initial)</td><td>1.0 g / m2/day</td><td>1.95 g / m2/day</td>

<td>Peeled (1 week)</td><td>5 pounds (2.3 kg)</td><td>20 lbs (9 kg)</td>

<td>Coating shear</td><td>6 psi (0.4</td><td>8 psi (0.6</td>

<td>to (initial)</td><td>kg / cm2)</td><td>kg / cm2)</td>

<td>Coating shear</td><td>7 psi (0.5</td><td>15 psi (1.0</td>

<td>Hardness (initial)</td><td>35 Shore A</td><td>35 Shore A</td>

<td>Hardness (1 month)</td><td>35 Shore A</td><td>58 Shore A</td>

<td>Block H (initial)</td><td>12.5 psi (0.9 kg / cm2)</td><td>14 psi (1.0 kg / cm2)</td>

<td>Block H (48 hours)</td><td>13.7 psi (0.96 kg / cm2)</td><td>40 psi (2.8 kg / cm2)</td>

<td>Module (initial)</td><td>Not measured</td><td>30-35 psi (2.12.5 kg / cm2)</td>

<td>Modulus (cured)</td><td>30 psi (2.1 kg / cm2)</td><td>35-100 psi (2.57 kg / cm2)</td>

ES 2 274 807 T3

The values in Table 6 were based on a proven sealant thickness of 1.5mm unless otherwise noted below. For the values in Table 6, the wet vapor transmission rate (MVT) was measured according to ASTM F 1249. Exfoliation resistance values were measured according to Sealed Insulating Glass Manufacturers Association (SIGMA) test method P.7.A using 3/16 inch (0.5 cm) by 1 inch ( 2.5 cm) by 5 inch (12.5 cm), a steel strip 0.010 inch (0.03 cm) by 1.0 inch (2.5 cm); 0.060 inch (0.15 cm) thick bead of sealant; and a crosshead speed of 2.0 inches per minute (5 cm / min). Coating shear strength values were determined using SIGMA's P.6.A test method using 3/16 inch by 1 inch by 2 inch (0.5 cm by 2.5 cm by 5 cm) glass pieces. cm); 0.060 inch (0.15 cm) sealant thickness; and a crosshead speed of 2.0 inches per minute (5 cm / min). Hardness was determined according to test procedure P.1.A, Initial Hardness Test, from SIGMA. The H block test was performed by placing three wooden blocks between two 3/16 inch (0.5 cm) pieces of 2 inch thick by 2 inch (5 cm by 5 cm) glass. The center block was 1/2 inch by 1/2 inch by 2 inch (1.3 cm by 1.3 cm by 5 cm). Masking tape was wrapped around the outside of the glass pieces to hold the blocks in position between the two glass pieces. The center block was then removed leaving a 1/2 inch by 1/2 inch by 2 inch (1.3 cm by 1.3 cm by 5 cm) channel through the center of the frame. The primary sealant from Example 3 was extruded into this center channel, slightly overfilling the channel. Excess material, ie material beyond the edges of the glass, was cut off and the sample was allowed to stand for one hour. The tape was removed and the two remaining wooden blocks between the glass sheets were removed. This left the two 2-inch by 2-inch (5 cm by 5 cm) glass plates connected at their longitudinal centers by a 1/2-inch by 1/2-inch by 2-inch (1.3 cm) block of sealant. by 1.3 cm by 5 cm). Tensile strength was tested using a commercial tensile strength apparatus, commercially available from Instron, Inc., to separate the glass pieces at a crosshead speed of 2 inches per minute (5 cm / min). . The values in Table 6 represent the load when the material failed. The modulus was determined according to ASTM D412.

Thus, the present invention provides a sealant material that is especially useful as a primary sealant for a double seal IG unit. As set forth in Table 6, the primary sealant of the invention has a wet vapor transmission rate (1.95 g / m2/ day) much lower than conventional thermoset materials (typically higher than 10 g / m2/ day) and is comparable to that of conventional PIB sealant (1.0 g / m2/day). In addition, the primary sealant of the invention has a higher modulus value (35-100 psi; 2.5-7 kg / cm2) than conventional GDP (30 psi; 2.1 kg / cm2), which promotes the structural integrity of the IG unit. However, the modulus value of the primary sealant material is generally less than that of conventional thermosets (typically greater than 200 psi; 14 kg / cm2) so that the primary sealant of the invention will not be excessively stressed if the IG unit flexes or twists during normal operation. Thus, the primary sealant of the invention provides a moisture vapor transmission rate comparable to that of a conventional thermoplastic material and also promotes the structural integrity of the IG unit.

Those skilled in the art will readily appreciate that modifications can be made to the invention without departing from the concepts described in the foregoing description. Accordingly, the particular embodiments described in detail herein are illustrative only and do not limit the scope of the invention, to which the full scope of the appended claims and any and all equivalents are to be given.

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15200899	United States of America	P	1999-09-01
15200899	United States of America	P	1999-09-01
19990152008P	United States of America	–	1999-09-01
00961543152008P	–	–	–
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CA2384189A1	Canada	A1	2001-03-08
WO0116046A1	World Intellectual Property Organization (WIPO)	A1	2001-03-08
AU7348400A	Australia	A	2001-03-26
NO20021055D0	Norway	D0	2002-03-01
NO20021055L	Norway	L	2002-05-02
KR20020042661A	Republic of Korea	A	2002-06-05
EP1216212A1	European Patent Office (EPO)	A1	2002-06-26
US6457294B1	United States of America	B1	2002-10-01
CN1377329A	China	A	2002-10-30
US2002194813A1	United States of America	A1	2002-12-26
JP2003508327A	Japan	A	2003-03-04
AU771280B2	Australia	B2	2004-03-18
US6796102B2	United States of America	B2	2004-09-28
EP1216212B1	European Patent Office (EPO)	B1	2006-11-15
AT345317T	Austria	T	2006-12-15
ATE345317T1	Austria	T1	2006-12-15
DE60031866D1	Germany	D1	2006-12-28
DK1216212T3	Denmark	T3	2007-03-19
KR100710534B1	Republic of Korea	B1	2007-04-24
DE60031866T2	Germany	T2	2007-05-31
ES2274807T3This record	Spain	T3	2007-06-01
CN100352783C	China	C	2007-12-05
CA2384189C	Canada	C	2008-04-15

Insulating glass unit with structural primary sealant system

Abstract

Term

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DESCRIPTION

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TABLE 2

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CQ

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TABLE 4

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TABLE 5

TABLE 6

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Priority claims5

Members23

Numbers

Titles2

Classification