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Composition Comprising Silylated Polymers and Polyhedral Oligomeric Metallo Silsesquioxane

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Composition Comprising Silylated Polymers and Polyhedral Oligomeric Metallo Silsesquioxane (19) TZZ ¥_T (11) EP 2 796 493 A1 (12) EUROPEAN PATENT APPLICATION (43) Date of publication: (51) Int Cl.: 29.10.2014 Bulletin 2014/44 C08K 5/549 (2006.01) C08L 43/04 (2006.01) C08G 18/22 (2006.01) (21) Application number: 13165285.1 (22) Date of filing: 25.04.2013 (84) Designated Contracting States: • Huntsman (Europe) BVBA AL AT BE BG CH CY CZ DE DK EE ES FI FR GB 3078 Everberg (BE) GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR (72) Inventor: The designation of the inventor has not Designated Extension States: yet been filed BA ME (74) Representative: Swinnen, Anne-Marie et al (71) Applicants: Huntsman (Europe) BVBA • HUNTSMAN INTERNATIONAL LLC Intellectual Property Department Salt Lake City, Utah 84108 (US) Everslaan 45 3078 Everberg (BE) (54) Composition comprising silylated polymers and polyhedral oligomeric metallo silsesquioxane (57) The present invention relates to a composition composition comprising a silylated polymer comprising comprising at least one silylated polymer and at least one the step of: contacting a silylated polymer with a polyhe- polyhedral oligomeric metallo silsesquioxane. The dral oligomeric metallo silsesquioxane. present invention also relates to a process of curing a EP 2 796 493 A1 Printed by Jouve, 75001 PARIS (FR) EP 2 796 493 A1 Description FIELD OF INVENTION 5 [0001] This invention relates to a composition comprising silylated polymers comprising alkoxysilyl and/or silanol moieties, and more specifically silylated polyurethanes and to a process to prepare such compositions. BACKGROUND OF THE INVENTION 10 [0002] Many commercial compositions containing moisture curable silylated polymers are known, and have many commercial applications. For example, silylated polyurethane resins are useful as coatings, adhesives, sealants and industrial elastomeric goods. [0003] The curing of these moisture curable silylated polymer compositions requires the use of curing agents. Organotin compounds (e.g. dibutyl tin dilaurate (DBTDL)) have proved to be the most effective compounds to catalyze the curing 15 process which comprises hydrolysis/condensation reactions of the silylated polymers. [0004] However, these organotin compounds are classified as toxic, and therefore, their use should be avoided or limited in articles for human or animal use. [0005] Therefore, there is a need for a curing agent, which can replace organotin compounds, and which displays at least similar performance levels compared to these compounds. 20 [0006] In the past problems related to the toxicity of tin have been addressed by limiting the quantities of tin in the final polymer, merely reducing the tin level below 0.1wt%. Alternatively, other organometallic curing agents based on e.g. Zr, Bi, Ti etc. have been screened. Also, pH driven cure processes using amines and/or acids as curing agents have been used for the silylated polymers. [0007] However, these alternatives have not proven to be satisfactory, either the tin levels are still too high from a 25 toxicity point of view or the alternative curing agents do not perform at the same level as tin. Furthermore, some alternative curing agents are known to result in strong discoloring of the polymer, which is not a desired feature. SUMMARY OF THE INVENTION 30 [0008] According to a first aspect of the present invention, a composition is provided, comprising at least one silylated polymer and at least one polyhedral oligomeric metallo silsesquioxane. [0009] According to a second aspect, the present invention also encompasses a process of curing a composition according to the first aspect of the invention, said process comprising the step of: contacting at least one silylated polymer with at least one polyhedral oligomeric metallo silsesquioxane; thereby obtaining a cured composition. 35 [0010] It has been now surprisingly found that the use of polyhedral oligomeric metallo silsesquioxane compounds (POMS) as a curing agent has demonstrated to increase the hydrolysis and condensation rate of organofunctional alkoxysilyl and/or silanol groups. Specifically, in silylated polymer systems, and more specifically in silylated polyurethane systems these curing agents have displayed an activity twice as high compared to organotin compounds in surface cure experiments. 40 [0011] The independent and dependent claims set out particular and preferred features of the invention. Features from the dependent claims may be combined with features of the independent or other dependent claims as appropriate. [0012] The above and other characteristics, features and advantages of the present invention will become apparent from the following detailed description, taken in conjunction with the accompanying drawings, which illustrate, by way of example, the principles of the invention. The reference figures quoted below refer to the attached drawings. 45 BRIEF DESCRIPTION OF THE DRAWINGS [0013] 50 Figure 1 represents a graph plotting Start Opening Times for catalysed silylated polyurethane resins as a function of wt% of catalyst. DETAILED DESCRIPTION OF THE INVENTION 55 [0014] Before the present compositions and formulations of the invention are described, it is to be understood that this invention is not limited to particular compositions and formulations described, since such compositions and formu- lation may, of course, vary. It is also to be understood that the terminology used herein is not intended to be limiting, since the scope of the present invention will be limited only by the appended claims. 2 EP 2 796 493 A1 [0015] As used herein, the singular forms "a", "an", and "the" include both singular and plural referents unless the context clearly dictates otherwise. [0016] The terms "comprising", "comprises" and "comprised of" as used herein are synonymous with "including", "includes" or "containing", "contains", and are inclusive or open-ended and do not exclude additional, non-recited mem- 5 bers, elements or method steps. It will be appreciated that the terms "comprising", "comprises" and "comprised of" as used herein comprise the terms "consisting of", "consists" and "consists of". [0017] The recitation of numerical ranges by endpoints includes all numbers and fractions subsumed within the re- spective ranges, as well as the recited endpoints. [0018] Allreferences cited in thepresent specification are hereby incorporated by referencein their entirety.In particular, 10 the teachings of all references herein specifically referred to are incorporated by reference. [0019] Unless otherwise defined, all terms used in disclosing the invention, including technical and scientific terms, have the meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. By means of further guidance, term definitions are included to better appreciate the teaching of the present invention. [0020] Whenever the term "substituted" is used in the present invention, it is meant to indicate that one or more 15 hydrogens on the atom indicated in the expression using "substituted" is replaced with a selection from the indicated group, provided that the indicated atom’s normal valency is not exceeded. [0021] Where groups may be optionally substituted, such groups may be substituted once or more, and preferably once, twice or thrice. Substituents may be selected from but are not limited to, for example, the group comprising alcohol, carboxylic acid, ester, amino, amido, ketone, ether and halide functional groups; such as for example halogen, hydroxyl, 20 oxo, amido, carboxy, amino, haloC1-6alkoxy, and haloC1-6alkyl. [0022] As used herein the terms such as "substituted or unsubstituted1-20 Calkyl", "substituted or unsubstituted C3-6cycloalkyl", "substituted or unsubstituted C2-20alkenyl", or "substituted or unsubstituted C6-10aryl" are synonymous to "C1-20alkyl, C3-6cycloalkyl, C2-20alkenyl, C6-10aryl, each being optionally substituted with... ". [0023] As used herein the terms such as "alkyl, alkenyl, aryl, or cycloalkyl, each being optionally substituted with..." 25 or "alkyl, alkenyl, aryl, or cycloalkyl, optionally substituted with .." encompasses "alkyl optionally substituted with...", "ar yl optionally substituted with..." and "cycloalkyl optionally substituted with...". [0024] The term "C1-24alkyl", as a group or part of a group, refers to a hydrocarbyl radical of Formula C nH2n+1 wherein n is a number ranging from 1 to 24. Preferably, the alkyl group comprises from 1 to 20 carbon atoms, for example 1 to 10 carbon atoms, for example 1 to 6 carbon atoms, for example 1 to 4 carbon atoms. Alkyl groups may be linear or 30 branched and may be substituted as indicated herein. When a subscript is used herein following a carbon atom, the subscript refers to the number of carbon atoms that the named group may contain. Thus, for example, C 1-20alkyl means an alkyl of 1 to 20 carbon atoms. Thus, for example, C 1-6alkyl means an alkyl of 1 to 6 carbon atoms. Examples of alkyl groups are methyl, ethyl, propyl, isopropyl (i-propyl), butyl, isobutyl (i-butyl),sec -butyl, tert-butyl, pentyl and its chain isomers, hexyl and its chain isomers. When the term "alkyl" is used as a suffix following another term, as in "hydroxyalkyl", 35 this isintended torefer to an alkylgroup, as defined above, being substitutedwith one or two (preferably one)substituent(s ) selected from the other, specifically-named group, also as defined herein. The term "hydroxyalkyl" therefore refers to a -Ra-OH group wherein Ra is alkylene as defined herein. [0025] The term "C 3-24cycloalkyl" as a group or
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