Crosslinkable composition based on an organosilicon compound

Abstract

The present invention relates to a crosslinkable composition that can be prepared using (A) an organopolysiloxane of the formula (R2O)3-aSiR1aO(SiR2O)nSiR1a(OR2)3-a(I) (provided that the viscosity at 25°C is 6000 mPas or more), (B1) a silane of the formula R34-b(R4O)bSi (II) [provided that the molecular weight of the silane of formula (II) is greater than 195 g / mol), and optionally (B2) a silicon compound composed of units of R7c(R8O)dSiO(4-cd) / 2(III) [provided that in formula (III), the sum c+d is 3 or less, at least two groups (R8O) are present in the silicon compound, and the viscosity at 25°C is less than 2000 mPas], wherein radicals and indexes have the meanings set forth in claim 1, provided that the composition The organopolysiloxane (A) contains an organosilicon compound having a molecular weight of 195 g / mol or less in an amount of less than 0.5 weight%. The present invention also relates to a method for preparing and using the above composition.

Description

Technology Field

[0001] The present invention relates to a composition based on an organosilicon compound and capable of being crosslinked by a condensation reaction, a method for manufacturing the same, and in particular, its use as a sealant for grouting natural stone. Background Technology

[0002] Alcohol-free, one-component sealants (RTV1 sealants) that can be stored in the absence of water and cure into an elastomer upon water penetration at room temperature are already known. Such products are used in large quantities, for example, in the construction industry. The basis of these mixtures is an organopolysiloxane having an alkoxy group as a hydrolyzable reactive substituent. Such reactive polydimethylsiloxanes are generally prepared by what is known as endcapping, which is the reaction of OH-terminated polydimethylsiloxane and organyloxysilane in the presence of a catalyst. In this regard, reference may be made to, for example, US-A 5,055,502. To suppress downstream reactions from endcapping (chain extension and crosslinking), organyloxysilane must always be used in a much greater excess compared to the OH groups of the OH-terminated polydimethylsiloxane. The result of this is that these organyloxypolymers always contain an excess of organyloxysilane. It was also revealed that, generally, terminal capping can be performed using highly reactive organyloxysilanes such as methyltrimethoxysilane or vinyltrimethoxysilane without equilibration.

[0003] Other reactive silanes also used are methyltriethoxysilane (MTEO) or vinyltriethoxysilane (VTEO). However, the reactivity of the latter two silanes is already too low, so there are limitations to their use for terminal blocking of long-chain OH-terminated polydimethylsiloxanes, as can be inferred from US-B2 10647822. Nevertheless, these silanes are actually used as additional additives, for example as water scavengers to increase storage stability, or as carrier materials for additional active ingredients, such as stabilizers or catalysts.

[0004] The profile of requirements imposed on RTV1 sealants is extensive, but there is a particular demand for products that cure very rapidly after a specific processing time. In addition to the catalyst used in RTV1 sealants, a decisive factor here is the reactivity of the crosslinking agent used. Specifically, commonly used tin and titanium compounds have disadvantages, such as causing storage stability issues or unwanted yellowing. Therefore, the issue is to limit the amount of catalyst used in RTV1 sealants. However, in this case, the pressure to use highly reactive silanes becomes much greater.

[0005] In addition, these sealants may include fillers, plasticizers, crosslinking agents, and various additives.

[0006] It is also common to use functionalized alkylsilanes called adhesion promoters. A typical example is the use of aminopropyltrimethoxysilane.

[0007] Of course, all these alkoxysilanes and methyltrimethoxysilanes additionally present in the RTV1 sealant can also affect curing properties such as skin formation time, early strength, and penetration curing. However, this effect is very small and generally negligible. However, when these silanes are used in the described RTV1 sealant, there are disadvantages that affect manufacturing, storage, and use.

[0008] One of the significant drawbacks of conventional RTV1 sealants is that substrates in contact with the sealant, particularly natural stone, can become contaminated during grouting scenarios. This is primarily caused by plasticizers that are not included in the polymer matrix. These plasticizers can migrate from the sealant and form dark-colored margins with an oily appearance in the areas in contact with the substrate.

[0009] A known solution to this problem is to use very short-chain plasticizers, as disclosed in DE-B 102 27 590. Nevertheless, it has been found that there is an additional type of contamination that appears only when the substrate is wet. The area in contact with the sealant is highly hydrophobic, so it does not get wet and appears in a much lighter color than the rest of the substrate. This phenomenon occurs regardless of the specific plasticizer used. It occurs even when no plasticizer is added at all.

[0010] In contrast to the highly reactive organyloxysilane described above, the high molecular weight organyloxysilane is characterized by low reactivity because it contains not only long-chain organyloxy radicals but also long-chain organyl radicals directly bonded to silicon.

[0011] The subject of the present invention is a composition capable of being crosslinked by a condensation reaction and prepared using the following (A), (B1) and optionally (B2), provided that the composition of the present invention contains an organosilicon compound having a molecular weight of 195 g / mol or less in an amount of less than 0.5 weight%, preferably less than 0.1 weight%, based on organopolysiloxane (A) in each case:

[0012] (A) Organopolysiloxane of the following chemical formula (I)

[0013] (R 2 O) 3-a SiR 1 a O(SiR2O) n SiR1 a (OR 2 ) 3-a (I)

[0014] (during the meal,

[0015] R may be the same or different and represents a monovalent, optionally substituted hydrocarbon radical, and

[0016] R 1 It may be the same or different and represents a monovalent, optionally substituted hydrocarbon radical, and

[0017] R 2 It may be the same or different and represents a monovalent, optionally substituted hydrocarbon radical, and

[0018] a may be the same or different, 0 or 1, preferably 1, and

[0019] n is an integer from 380 to 2000, and

[0020] However, the viscosity at 25℃ is 6000 mPas or higher.)

[0021] (B1) Silane of the following chemical formula (II)

[0022] R 3 4-b (R 4 O) b Si (II)

[0023] (during the meal,

[0024] R 3 It may be the same or different and represents a monovalent, SiC-bonded, optionally substituted hydrocarbon radical, and

[0025] R 4 It may be the same or different and represents a monovalent, optionally substituted hydrocarbon radical, and

[0026] b is 2, 3, or 4, preferably 2 or 3, and

[0027] However, the molecular weight of the silane of chemical formula (II) is greater than 195 g / mol.)

[0028] (B2) Silicon compounds composed of units of the following chemical formula (III)

[0029] R 7 c (R 8 O) d SiO (4-c-d) / 2 (III)

[0030] (during the meal,

[0031] R 7 It may be the same or different and represents a monovalent, SiC-bonded, optionally substituted hydrocarbon radical, and

[0032] R 8 It may be the same or different and represents a monovalent, optionally substituted hydrocarbon radical, and

[0033] c is 0, 1, or 2, and

[0034] d is 0, 1, 2, or 3, and

[0035] Provided that in chemical formula (III), the sum of c+d is ≤3, and at least two groups (R) in the silicon compound 8 O) is present, and the viscosity at 25℃ is less than 2000 mPas.) Specific details for implementing the invention

[0036] Examples of radical R include alkyl radicals such as methyl, ethyl, n-propyl, isopropyl, 1-n-butyl, 2-n-butyl, isobutyl, tert-butyl, n-pentyl, isopentyl, neopentyl, and tert-pentyl radicals; hexyl radicals such as n-hexyl radicals; heptyl radicals such as n-heptyl radicals; octyl radicals such as n-octyl radicals and isooctyl radicals such as 2,2,4-trimethylpentyl radicals; nonyl radicals such as n-nonyl radicals; decyl radicals such as n-decyl radicals; dodecyl radicals such as n-dodecyl radicals; and octadecyl radicals such as n-octadecyl radicals. Cycloalkyl radicals such as cyclopentyl, cyclohexyl, cycloheptyl radicals and methylcyclohexyl radicals; alkenyl radicals such as vinyl, 1-propenyl, and 2-propenyl radicals; aryl radicals such as phenyl, naphthyl, anthryl, and phenanthryl radicals; alkaryl radicals such as o-, m-, and p-tolyl radicals; xylyl radicals and ethylphenyl radicals; and aralkyl radicals such as benzyl radicals, α- and β-phenylethyl radicals.

[0037] Radical R is preferably a monovalent hydrocarbon radical having 1 to 18 carbon atoms, more preferably a methyl, vinyl, or phenyl radical, more particularly a methyl radical.

[0038] Radical R 1 Examples of are the monovalent hydrocarbon radicals indicated for R and also hydrocarbon radicals substituted with amino groups.

[0039] Radical R 1 It preferably comprises a monovalent hydrocarbon radical having 1 to 12 carbon atoms and optionally substituted by an amino group, and more preferably a methyl radical, ethyl radical, vinyl radical, phenyl radical, or radical -CH2-NR 6' R 5' or radical CH2NR 11' Includes, where R 5' represents a hydrocarbon radical having 1 to 12 carbon atoms, and R6' is a hydrogen atom or R 5' Represents a radical, R 11' represents a divalent hydrocarbon radical in which a heteroatom can be interposed.

[0040] More specifically, radical R 1 Silver radical -CH2-NR 6' R 5' or radical CH2NR 11' Includes, where R 5' , R 6' and R 11' It has the same meaning as mentioned above and very preferably includes -CH2-N[(CH2)2]2O, -CH2-N(Bu)2 or -CH2-NH(cHex), where Bu represents an n-butyl radical and cHex represents a cyclohexyl radical.

[0041] Radical R 5 and R 5' Examples are hydrocarbon radicals expressed independently for R.

[0042] Preferably radical R 5 and R 5' It independently comprises methyl, ethyl, isopropyl, n-propyl, n-butyl, cyclohexyl, or phenyl radicals, more preferably n-butyl radicals.

[0043] Hydrocarbon radical R 6 and R 6' Examples are hydrocarbon radicals expressed independently for R.

[0044] Preferably radical R 6 and R 6' It independently comprises hydrogen atoms, methyl, ethyl, isopropyl, n-propyl, n-butyl, or cyclohexyl radicals, more preferably n-butyl radicals.

[0045] divalent radical R 11 and R 11'Examples of which are independently alkylene radicals such as propane-1,3-diyl, butane-1,4-diyl, butane-1,3-diyl, 2-methylpropane-1,3-diyl, pentane-1,5-diyl, pentane-1,4-diyl, 2-methylbutane-1,4-diyl, 2,2-dimethylpropane-1,3-diyl, hexane-1,6-diyl, heptane-1,7-diyl, octane-1,8-diyl and 2-methylheptane-1,7-diyl and 2,2,4-trimethylpentane-1,5-diyl radicals; alkenylene radicals such as propene-1,3-diyl radicals; and also -CH2-CH2-O-CH2-CH2- and -CH2-CH2-NH-CH2-CH2-.

[0046] Radical R 11 and R 11' It comprises divalent hydrocarbon radicals having 4 to 6 carbon atoms that can be independently interposed, preferably by heteroatoms, preferably oxygen -O- or nitrogen -NH-, and more preferably CH2-CH2-O-CH2-CH2-.

[0047] Radical R 2 An example is a monovalent radical represented for R.

[0048] Radical R 2 It preferably comprises an alkyl radical having 1 to 12 carbon atoms, more preferably a methyl, ethyl, n-propyl, or isopropyl radical, more particularly a methyl or ethyl radical.

[0049] The organopolysiloxane (A) used in the present invention is preferably

[0050] (MeO)2Si(Ox)O(SiMe2O) 30-2000 Si(Ox)(OMe)2,

[0051] (MeO)2Si(DBA)O(SiMe2O) 30-2000 Si(DBA)(OMe)2,

[0052] (MeO)2Si(cHx)O(SiMe2O) 30-2000 Si(cHx)(OMe)2,

[0053] (MeO)2Si(R 3 )O(SiMe2O) 700 Si(R 3 )(OMe)2,

[0054] (EtO)2Si(Ox)O(SiMe2O) 30-2000 Si(Ox)(OEt)2,

[0055] (EtO)2Si(DBA)O(SiMe2O) 30-2000 Si(DBA)(OEt)2,

[0056] (EtO)2Si(cHx)O(SiMe2O) 30-2000 Si(cHx)(OEt)2 or

[0057] (EtO)2Si(R 1 )O(SiMe2O) 700 Si(R 1 )(OEt)2, more preferably

[0058] (EtO)2Si(Ox)O(SiMe2O) 30-2000 Si(Ox)(OEt)2,

[0059] (EtO)2Si(DBA)O(SiMe2O) 30-2000 Si(DBA)(OEt)2 or

[0060] (EtO)2Si(cHx)O(SiMe2O) 30-2000 Si(cHx)(OEt)2, more preferably

[0061] (EtO)2Si(Ox)O(SiMe2O) 30-2000 Si(Ox)(OEt)2

[0062] It includes, where Me is a methyl radical, Et is an ethyl radical, Ox is CH2-N[(CH2)2]2O, DBA is -CH2-N(nBu)2, cHx is CH2-NH(cHex), Bu is an n-butyl radical, cHex is a cyclohexyl radical, and also R 1 represents Me, Et, vinyl radical, phenyl radical, DBA, Ox, or cHx, and has the same meaning within individual compounds.

[0063] The organopolysiloxane (A) used in the present invention has a viscosity of preferably 6,000 to 350,000 mPas, more preferably 20,000 to 120,000 mPas, at 25°C in each case.

[0064] Organopolysiloxane (A) is a commercially common product and / or can be manufactured by conventional methods in silicon chemistry.

[0065] Radical R 3 An example is a radical represented for R.

[0066] Radical R 3 The radical is preferably a linear, branched, or cyclic hydrocarbon radical having 1 to 16 carbon atoms, or a monovalent hydrocarbon radical having 1 to 12 carbon atoms substituted with an amino group on a carbon atom bonded to a silicon atom, and more preferably a linear, branched, or cyclic alkyl radical, vinyl radical, phenyl radical, or radical -CH2-NR having 1 to 8 carbon atoms. 6' R 5' or radical CH2NR 11' and, here, R 5' represents a hydrocarbon radical having 1 to 12 carbon atoms, and R 6' is a hydrogen atom or radical R 5' Represents, and R 11' represents a divalent hydrocarbon radical in which a heteroatom can be interposed.

[0067] Radical R 4 An example is a radical represented for R.

[0068] Preferably radical R 4 is a methyl, ethyl, n-propyl, isopropyl, n-butyl, s-butyl, or isobutyl radical, more preferably an ethyl, n-propyl, or isopropyl radical.

[0069] Examples of components (B1) optionally used in the present invention include n-hexyltrimethoxysilane, n-heptyltrimethoxysilane, n-octyltrimethoxysilane, n-nonyltrimethoxysilane, n-decyltrimethoxysilane, n-hexadecyltrimethoxysilane, cyclohexyltrimethoxysilane, phenyltrimethoxysilane, n-propyltriethoxysilane, n-butyltriethoxysilane, pentyltriethoxysilane, n-hexyltriethoxysilane, n-heptyltriethoxysilane, n-octyltriethoxysilane, n-nonyltriethoxysilane, n-decyltriethoxysilane, n-hexadecyltriethoxysilane, cyclohexyltriethoxysilane, phenyltriethoxysilane, methyltri-n-propoxysilane, ethyltri-n-propoxysilane, n-propyltri-n-propoxysilane, n-butyltri-n-propoxysilane, n-pentyltri-n-propoxysilane, n-hexyltri-n-propoxysilane, n-heptyltri-n-propoxysilane, n-octyltri-n-propoxysilane, n-nonyltri-n-propoxysilane, n-decyltri-n-propoxysilane, n-hexadecyltri-n-propoxysilane, cyclohexyltri-n-propoxysilane, phenyltri-n-propoxysilane, methyltriisopropoxysilane, ethyltriisopropoxysilane, n-propyltriisopropoxysilane, n-butyltriisopropoxysilane, n-pentyltriisopropoxysilane, n-hexyltriisopropoxysilane, n-heptyltriisopropoxysilane, n-octyltriisopropoxysilane, n-nonyltriisopropoxysilane, n-decyltriisopropoxysilane, n-hexadecyltriisopropoxysilane, cyclohexyltriisopropoxysilane, phenyltriisopropoxysilane, 2,2,4-trimethylpentyltrimethoxysilane, tetraethoxysilane, tetra-n-propoxysilane, tetraisopropoxysilane, 2,2,4-trimethylpentyltriethoxysilane, (2,3,5,6-tetrahydro-1,4-oxazine-4-yl)methyltriethoxysilane, N,N-di-n-butylaminomethyltriethoxysilane, N-cyclohexylaminomethyltriethoxysilane, (2,3,5,6-tetrahydro-1,4-oxazine-4-yl)methyltrimethoxysilane, They are N,N-di-n-butylaminomethyltrimethoxysilane and N-cyclohexylaminomethyltrimethoxysilane.

[0070] Preferably, the silane (B1) used in the present invention is tetraethoxysilane, 2,2,4-trimethylpentyltrimethoxysilane, (2,3,5,6-tetrahydro-1,4-oxazine-4-yl)methyltriethoxysilane, phenyltrimethoxysilane, or n-hexadecyltrimethoxysilane.

[0071] The component (B1) may include commercially common products or be produced by conventional methods in silicon chemistry.

[0072] The composition of the present invention comprises, in each case, component (B1) in an amount preferably from 0.5 to 7 parts by weight, more preferably from 1 to 3.5 parts by weight, based on 100 parts by weight of component (A).

[0073] Radical R 7 An example is a radical represented for R.

[0074] Radical R 7 It is preferably a methyl radical or a 2,2,4-trimethylpentyl radical.

[0075] Radical R 8 An example is a radical represented for R.

[0076] Radical R 8 It is preferably a methyl radical or an ethyl radical, more preferably a methyl radical.

[0077] A preferred example of a silicon compound (B2) optionally used in the present invention is

[0078] EtO(SiMe2O)3SiR 7 (OEt)2,

[0079] (EtO(SiMe2O)3)2SiR 7 (OEt),

[0080] MeO(SiMe2O)3SiR 7 (OMe)2,

[0081] (MeO(SiMe2O)3)2SiR 7 OMe),

[0082] EtO(SiMe2O)3SiR 7 (OEt)O(SiMe2O)3SiR 7 (OEt)2,

[0083] MeO(SiMe2O)3SiR 7 (OMe)O(SiMe2O)3SiR 7 (OMe)2,

[0084] EtO(SiMe2O) x Si(iOct)(OEt)2,

[0085] (EtO(SiMe2O) x )2Si(iOct)(OEt),

[0086] MeO(SiMe2O) x Si(iOct)(OMe)2,

[0087] (MeO(SiMe2O) x )2Si(iOct)(OMe),

[0088] EtO(SiMe2O) x Si(iOct)(OEt)O(SiMe2O)3Si(iOct)(OEt) 2,

[0089] MeO(SiMe2O) x Si(iOct)(OMe)O(SiMe2O)3Si(iOct)(OMe) 2,

[0090] [(EtO)3SiO 1 / 2 ][(EtO)2SiO 2 / 2 ][(EtO)SiO 3 / 2 ][SiO 4 / 2 ] or

[0091] [(EtO)2SiMeO 1 / 2 ][(EtO)SiMeO 2 / 2 ][MeSiO 3 / 2 ]

[0092] , where Me is a methyl radical, Et is an ethyl radical, iOct is a 2,2,4-trimethylpentyl radical, x=1-9, and R 7 represents a straight-chain, branched, or cyclic aliphatic hydrocarbon radical having 2 to 8 carbon atoms, and radical R 7It has the same definition within individual compounds.

[0093] The silicon compound (B2) optionally used in the present invention is more preferably

[0094] MeO(SiMe2O) x Si(iOct)(OMe)2, (MeO(SiMe2O) x )2Si(iOct)(OMe),

[0095] MeO(SiMe2O) x Si(iOct)(OMe)O(SiMe2O)3Si(iOct)(OMe)2,

[0096] [(EtO)3SiO 1 / 2 ] 0.37 [(EtO)2SiO 2 / 2 ] 0.41 [(EtO)SiO 3 / 2 ] 0.20 [SiO 4 / 2 ] 0.02 or

[0097] [(EtO)2SiMeO 1 / 2 ] 0.18 [(EtO)SiMeO 2 / 2 ] 0.48 [MeSiO 3 / 2 ] 0.34

[0098] And, where Me is a methyl radical, Et is an ethyl radical, iOct is a 2,2,4-trimethylpentyl radical, and x = 1-9.

[0099] The silicon compound (B2) optionally used in the present invention preferably has a viscosity of 5 to 15 mPas at 25°C.

[0100] The silicon compound (B2) optionally used in the present invention preferably has a molecular weight greater than 195 g / mol.

[0101] More specifically, the silicon compound (B2) used arbitrarily has an average composition

[0102] [R 7 (OMe)2O 1 / 2 ] e [R 7 Si(OMe)O 2 / 2 ] f [R 7 SiO 3 / 2 ] g [Me2SiO 2 / 2 ] h [Me2Si(OMe)O 1 / 2 ] i

[0103] It has, where e=0.05-0.15, f=0.10-0.20, g=0.00-0.10, h=0.40-0.65 and i= 0.10-0.30, e+f+g < h+i and e+f+g+h+i=1, Me is a methyl radical, and R 7 ...has the definition described above.

[0104] The silicon compound (B2) used optionally can be prepared by a conventional method in silicon chemistry, for example, by equilibrating polydimethylsiloxane and trialkoxysilane under a basic catalyst.

[0105] When the composition of the present invention includes component (B2), the amount thereof is preferably 1 to 20 parts by weight, more preferably 1 to 10 parts by weight, and more particularly 2 to 6 parts by weight, based on 100 parts by weight of component (A) in each case.

[0106] In addition to components (A), (B1) and optionally (B2), the composition of the present invention may include all materials currently used in compositions crosslinkable by condensation reaction, such as an adhesion promoter (C), a curing promoter (D), a plasticizer (E), a filler (F), and an additive (G).

[0107] The adhesion promoter (C) used can be any adhesion promoter used so far in a crosslinkable composition by a condensation reaction.

[0108] Preferably, the adhesion promoter (C) comprises an organyloxysilane having a glycidyloxy, amino, ureido, acryloyloxy, or methacryloyloxy group, and also a partial condensate thereof.

[0109] Examples of adhesion promoters (C) are 3-aminopropyltrimethoxysilane, 3-aminopropyltrimethoxysilane, 3-(2-aminoethyl)aminopropyltrimethoxysilane, 3-(2-aminoethyl)aminopropyltriethoxysilane, 3-glycidyloxypropyltrimethoxysilane, 3-glycidyloxypropyltriethoxysilane, 3-methacryloyloxypropyltrimethoxysilane, 3-methacryloyloxypropyltriethoxysilane, 3-ureidopropyltrimethoxysilane, 3-ureidopropyltriethoxysilane, 3-aminopropyldimethoxymethylsilane, 3-aminopropyldiethoxymethylsilane, 3-(2-aminoethyl)aminopropyldimethoxymethylsilane and 3-(2-aminoethyl)aminopropyldiethoxymethylsilane.

[0110] When the composition of the present invention includes an adhesion promoter (C), the amount involved is preferably 0.5 to 5.0 parts by weight, more preferably 1 to 3 parts by weight, based on 100 parts by weight of component (A) in each case.

[0111] The curing accelerator (D) used can be any curing accelerator used to date in a crosslinkable composition by a condensation reaction.

[0112] Examples of curing accelerators (D) are titanium compounds such as titanium chelates such as tetrabutyl or tetraisopropyl titanate, or bis(ethylacetoacetate)diisobutoxytitanium, or organotin compounds such as di-n-butyltin dilaurate and di-n-butyltin diacetate, di-n-butyltin oxide, dimethyltin diacetate, dimethyltin dilaurate, dimethyltin dineodecanoate, dimethyltin oxide, di-n-octyltin diacetate, di-n-octyltin dilaurate, and di-n-octyltin oxide, and also reaction products of these compounds with alkoxysilanes such as the reaction product of di-n-butyltin diacetate and tetraethoxysilane, preferably di-n-octyltin diacetate, di-n-octyltin dilaurate, and di-octyltin oxide. The reaction product of di-n-octyltin oxide and tetraethoxysilane is tetrabutyl titanate, tetraisopropyl titanate, or bis(ethylacetoacetate)diisobutoxytitanium.

[0113] When the composition of the present invention includes a curing accelerator (D), the amount involved is preferably 0.001 to 20 parts by weight, more preferably 0.001 to 1 part by weight, based on 100 parts by weight of component (A) in each case.

[0114] Examples of plasticizers (E) that are optionally used include dimethylpolysiloxane that is liquid at room temperature and has a viscosity in the range of 5 to 1000 mPas, particularly at 25°C, which is terminally blocked by trimethylsiloxy groups, and also high-boiling point hydrocarbons such as liquid paraffin or mineral oil composed of, for example, naphthenic and paraffinic units.

[0115] When the composition of the present invention comprises component (E), the amount involved is, in each case, preferably 5 to 30 parts by weight, more preferably 5 to 25 parts by weight, based on 100 parts by weight of siloxane (A). The composition of the present invention preferably does not contain any plasticizer (E).

[0116] The filler (F) optionally used in the compound of the present invention may be any desired filler known to date.

[0117] Examples of optionally used fillers (F) include quartz, diatomaceous earth, calcium silicate, zirconium silicate, zeolite, metal oxide powders, such as aluminum oxide, titanium oxide, iron oxide or zinc oxide and / or mixtures thereof, barium sulfate, calcium carbonate, gypsum, silicon nitride, silicon carbide, boron nitride, glass powder, and plastic powders such as polyacrylonitrile powder. 2 Non-reinforced filler (F) having a BET surface area of ​​0.5g / g or less; 20 m carbon black and settling choke such as furnace black and acetylene black 2 Reinforcing fillers having a BET surface area greater than 1 / g; silica such as exothermically generated silica and precipitated silica; and fibrous fillers such as plastic fibers.

[0118] The filler (F) used optionally is preferably calcium carbonate or silica, more preferably silica or a mixture of silica and calcium carbonate.

[0119] The desired calcium carbonate product (F) is ground or precipitated and optionally surface-treated with a fatty acid such as stearic acid or a salt thereof. The desired silica is preferably pyrogenic silica.

[0120] When the composition of the present invention comprises a filler (F), the amount in question is, in each case, preferably 10 to 150 parts by weight, more preferably 10 to 130 parts by weight, and more particularly 10 to 100 parts by weight, based on 100 parts by weight of organopolysiloxane (A). The composition of the present invention preferably comprises a filler (F).

[0121] Examples of additives (G) are pigments, dyes, deodorizers, oxidation inhibitors, agents affecting electrical properties such as conductive carbon black, flame retardants, light stabilizers, biocides such as fungicides, bactericides and acaricides, cell-generating agents such as azodicarbonamide, heat stabilizers, scavengers such as Si-N containing silazane or silylamide, such as N,N'-bistrimethylsilylurea or hexamethyldisilazane, Lewis and Brønsted acids such as sulfonic acid, phosphoric acid, phosphoric acid esters, phosphonic acid and phosphonic acid esters, co-catalysts such as hydrogenated castor oil or polyethylene glycol terminated with OH on one or both sides, agents for further adjustment of modulus such as polydimethylsiloxane having OH terminal groups, and any desired siloxane different from components (A), (B) and (C).

[0122] When the composition of the present invention comprises an additive (G), the amount in question is, in each case, preferably 0.1 to 20 parts by weight, more preferably 0.1 to 15 parts by weight, and more particularly 0.1 to 10 parts by weight, based on 100 parts by weight of organopolysiloxane (A). The composition of the present invention preferably comprises component (G).

[0123] The individual components of the composition of the present invention may, in each case, be one of these components or a mixture of at least two of these components.

[0124] The composition of the present invention is preferably prepared without using any components other than components (A) to (G).

[0125] The composition of the present invention is preferably

[0126] (A) Organopolysiloxane of chemical formula (I),

[0127] (B1) Silane of chemical formula (II),

[0128] (B2) A silicon compound composed of units of chemical formula (III),

[0129] Optionally (C) adhesion promoter,

[0130] Optionally (D) curing accelerator,

[0131] Optional (E) plasticizer,

[0132] Optionally (F) filler, and

[0133] Optional (G) additives

[0134] It is a composition that can be manufactured using

[0135] The composition of the present invention is more preferably

[0136] (A) Organopolysiloxane of chemical formula (I),

[0137] (B1) Silane of chemical formula (II),

[0138] (B2) A silicon compound composed of units of chemical formula (III),

[0139] (C) Adhesion promoter,

[0140] Optionally (D) curing accelerator,

[0141] Optional (E) plasticizer,

[0142] Optionally (F) filler, and

[0143] Optional (G) additives

[0144] It is a composition that can be manufactured using

[0145] The composition of the present invention is more particularly

[0146] (A) Organopolysiloxane of chemical formula (I),

[0147] (B1) Silane of chemical formula (II),

[0148] (B2) A silicon compound composed of units of chemical formula (III),

[0149] (C) Adhesion promoter,

[0150] (D) Curing accelerator,

[0151] Optional (E) plasticizer,

[0152] (F) Filler, and

[0153] Optional (G) additives

[0154] It is a composition that can be manufactured using

[0155] In another preferred embodiment, the composition of the present invention is

[0156] (A) Organopolysiloxane of chemical formula (I),

[0157] (B1) Silane of chemical formula (II),

[0158] (B2) A silicon compound composed of units of chemical formula (III),

[0159] (C) Adhesion promoter,

[0160] (D) Curing accelerator,

[0161] (F) Filler, and

[0162] Optional (G) additives

[0163] A composition that can be manufactured using, provided that (E) it does not contain a plasticizer.

[0164] In a further preferred embodiment, the composition of the present invention is

[0165] (A) Organopolysiloxane of chemical formula (I),

[0166] (B1) Silane of chemical formula (II),

[0167] (B2) Siloxane composed of units of chemical formula (III),

[0168] (C) Adhesion promoter,

[0169] (D) Curing accelerator,

[0170] (F) Filler, and

[0171] (G) Additives

[0172] A composition that can be manufactured using, provided that (E) it does not contain a plasticizer.

[0173] To prepare the composition of the present invention, all components may be mixed with each other in any order. This mixing may take place at room temperature and ambient atmospheric pressure, i.e., about 900 to 1100 hPa. However, if desired, this mixing may also take place at a higher temperature, such as a temperature in the range of, for example, 35 to 135°C. Additionally, to remove volatile compounds or air, it is possible to perform mixing temporarily or continuously under reduced pressure, such as an absolute pressure of, for example, 30 to 500 hPa.

[0174] The mixing of the present invention is preferably carried out in the absence of water, that is, using raw materials having a moisture content preferably less than 10,000 mg / kg, more preferably less than 5,000 mg / kg, and more particularly less than 1,000 mg / kg. The mixing operation is preferably carried out by blanketing using dry air or an inert gas such as nitrogen with a corresponding gas having a moisture content preferably less than 10,000 μg / kg, more preferably less than 1,000 μg / kg, and more particularly less than 500 μg / kg. After preparation, the composition is preferably distributed into commercially conventional moisture-proof containers such as cartridges, tubular pouches, buckets, and drums.

[0175] In one preferred procedure, the first components (A), (B), optionally (C) and (E) are mixed together, optional filler (F) is added, and finally optional additional components (D) and (G) are added, and the temperature during mixing preferably does not exceed 60°C.

[0176] A further subject of the present invention is a method for preparing the composition of the present invention by mixing individual components.

[0177] The method of the present invention may occur continuously, in batches, or in semi-batches using a known apparatus according to a known process.

[0178] The composition of the present invention and / or the composition prepared according to the present invention can be stored in a moisture-free state and can be crosslinked upon moisture penetration.

[0179] The typical moisture content of air is sufficient to crosslink the composition of the present invention. The composition of the present invention is preferably crosslinked at room temperature. If desired, it is crosslinked at a temperature higher or lower than room temperature, e.g., -5°C to 15°C or 30°C to 50°C, and / or through a water concentration exceeding the normal moisture content of air.

[0180] The crosslinking is preferably performed at a pressure of 100 to 1100 hPa, more particularly at ambient atmospheric pressure, i.e., about 900 to 1100 hPa.

[0181] A further subject of the present invention is a molded article manufactured by crosslinking the composition of the present invention.

[0182] The molded article of the present invention has a stress at 100% elongation of preferably less than 0.4 MPa when measured on an ISO 37 Type 2 test specimen.

[0183] The composition of the present invention can be used for any purpose in which a composition that can be stored in the absence of water and crosslinks to an elastomer upon water penetration at room temperature is available.

[0184] Surprisingly, it was found that by exclusively using silanes with a molecular weight greater than 195 g / mol, a sealant with excellent reactivity and high storage stability could be produced.

[0185] Surprisingly, it was further demonstrated that crosslinkable compositions based solely on high molecular weight silanes do not cause marginal contamination affecting natural stone grouting, even when they do not simultaneously contain inert plasticizers. It was not expected that these unwanted effects could be completely avoided through a relatively small increase in molecular weight. On the contrary, those skilled in the art would have expected that, due to lower reactivity, higher molecular weight alkoxysilanes would require more time to diffuse out of the RTV1 sealant during the sealant curing process. Therefore, the impact of marginal contamination resulting from the hydrophobization of the natural stone surface tended to be intensified, particularly because longer alkyl radicals further increase the hydrophobization effect.

[0186] Accordingly, the composition of the present invention has excellent suitability as a sealing compound for joints having a transparent width of, for example, 10 to 40 mm, including vertical joints and similar cavities, in the manufacture of window structures or display cases, for example, for surfaces exposed to continuous action of fresh or salt water, or in the manufacture of protective coatings or elastomer moldings.

[0187] The advantage of the composition of the present invention is that it is easy to manufacture and is characterized by very high storage stability.

[0188] Another advantage of the composition of the present invention is that it exhibits excellent handling quality during use and has excellent processing characteristics in various applications.

[0189] An advantage of the crosslinkable composition of the present invention is that the modulus can be customized.

[0190] The advantage of the crosslinkable composition of the present invention is that it adheres very well to a number of substrates.

[0191] An advantage of the crosslinkable composition of the present invention is that it does not cause marginal contamination of adjacent substrates. In particular, it has excellent suitability for grouting natural and artificial stones without marginal contamination.

[0192] The advantage of the crosslinkable composition of the present invention is that it is very economical in terms of the materials used.

[0193] In the embodiments described below, all viscosity data are associated with a temperature of 25°C. Unless otherwise indicated, the embodiments below are performed at ambient atmospheric pressure, i.e., about 1000 hPa, and room temperature, i.e., about 23°C or the temperature at which the reactants react, or at room temperature without additional heating or cooling, with a relative atmospheric humidity of about 50%. Additionally, unless otherwise specified, all part and percentage data are associated with weight.

[0194] Tensile strength, elongation at break, and stress at 100% elongation are determined according to ISO 37 for Type 2 test specimens.

[0195] In the context of the present invention, the dynamic viscosity of organosilicon compounds is measured according to DIN 53019. The procedure for this is as follows: Unless otherwise indicated, viscosity is measured at 25°C using an Anton Paar Physica MCR 300 rotary rheometer. For viscosities between 1 and 200 mPa·s, a coaxial cylinder measuring system (CC 27) with an annular measuring interval of 1.13 mm is used, whereas for viscosities exceeding 200 mPa·s, a cone / plate measuring system (Searle system with CP50-1 measuring cone) is used. The shear rate is the polymer viscosity (100 s -1 At 1 to 99 mPa·s; 200 s -1 At 100 to 999 mPa·s; 120 s -1 At 1000 to 2999 mPa·s; 80 s -1 At 3000 to 4999 mPa·s; 62 s-1 at 5000 to 9999 mPa·s; 50 s -1 At 10,000 to 12,499 mPa·s; 38.5 s -1 At 12,500 to 15,999 mPa·s; 33 s -1 At 16,000 to 19,999 mPa·s; 25 s -1 From 20,000 to 24,999 mPa·s; 20 s -1 From 25,000 to 29,999 mPa·s; 17 s -1 From 30,000 to 39,999 mPa·s; 10 s -1 From 40,000 to 59,999 mPa·s; 5 s -1 from 60,000 to 149,999; 3.3 s -1 From 150,000 to 199,999 mPa·s; 2.5 s -1 From 200,000 to 299,999 mPa·s; 1.5 s -1 It is 300,000 to 1,000,000 mPa·s).

[0196] In the context of the present invention, the number average and weight average molecular weights Mn and Mw are determined as follows:

[0197] Method: Size exclusion chromatography (SEC) according to DIN 55672-1

[0198] Flow rate: 1.00 mL / min

[0199] Injection System: Agilent 1200 Autosampler (Agilent Technologies)

[0200] Injection volume: 100 µl

[0201] Eluent: For products containing phenyl groups, >99.5% tetrahydrofuran was used and stabilized with 250 ppm 2,6-di-tert-butyl-4-methylphenol (BHT); for substances not containing phenyl groups, >99.9% analytical grade toluene was used. All chemicals are commercially available, for example, from Merck KGaA, D-Darmstadt (DE).

[0202] Column: Stationary phase: Polystyrene-divinylbenzene from Agilent Technologies.

[0203] Four columns were connected in series, each consisting of a 50 mm long pre-column and three separation columns, each 300 mm long. The inner diameter of all columns was 7.8 mm. The particle size of the gel used was 5 µm. The pore size of the pre-column was 500 Å, and the pore sizes of the three separation columns were 10,000 Å, 500 Å, and 100 Å, respectively.

[0204] Column temperature: Oven temperature 45℃. Concentration was determined using an RI detector (Measurement principle: Deflection, Type: Agilent 1200; Cell volume: 8 µL; Temperature: 45℃).

[0205] Similarly, the system was calibrated using a commercially available polystyrene standard from Agilent. Concentration: 0.4 g / L (EasiCal, commercially available polystyrene calibrator; injection volume: 100 µL). Tetrahydrofuran was used as the marker material for the internal standard for the eluent toluene, and toluene was used as the marker material for the internal standard for the eluent tetrahydrofuran. Calibration curve fitting: 3rd-order polynomial Fit PSS.

[0206] Sample preparation: Approximately 15–50 mg of the sample to be measured was dissolved in each eluent (c = approximately 3–10 mg / mL). The sample volumes were prepared to obtain a distinct RI signal. All samples were completely dissolved in the eluent.

[0207] Evaluation: The measured molar weights were rounded to the nearest whole bag in each case.

[0208] Marginal contamination of porous substrates was measured according to ASTM (American Society for Testing and Materials) C 1248. Specimens consisting of sealant and sandstone were vulcanized at 23°C and 50% relative humidity for 21 days, followed by 25% compression, for a total of 28 days.

[0209] 1) At 23℃ and 50% relative humidity,

[0210] 2) In a heat cabinet at 70℃, and

[0211] 3) In a UV test chamber as described in ASTM C 1248

[0212] Stored.

[0213] Next, marginal contamination was evaluated visually. If there was no visible marginal contamination, the result was 0 mm. When marginal contamination was determined, the maximum width (mm) of the area showing the greatest contamination was reported, rounded to an integer.

[0214] In the examples below, all mixtures were produced in a Labmax planetary mixer.

[0215] Example 1

[0216] Preparation of Siloxane A1

[0217] A mixture of 660 g of α,ω-dihydroxypolydimethylsiloxane with a viscosity of 80,000 mPas and 220 g of α,ω-dihydroxypolydimethylsiloxane with a viscosity of 20,000 mPas was stirred at 200 rotations / min for 5 minutes with 30.44 g of a solution of 0.04 g of 1,5,7-triazabicyclo[4.4.0]dex-5-ene in 30.4 g of (2,3,5,6-tetrahydro-1,4-oxazine-4-yl)methyltriethoxysilane. After a reaction time of 5 minutes, a mixture of 98.0 wt% α,ω-bis((2,3,5,6-tetrahydro-1,4-oxazine-4-yl)methyldiethoxysilyl)polydimethylsiloxane, 1.9 wt% (2,3,5,6-tetrahydro-1,4-oxazine-4-yl)methyltriethoxysilane, and 0.1 wt% ethanol with a viscosity of 52,000 mPas was obtained.

[0218] Preparation of Mixture M1

[0219] 455 g of the reaction mixture obtained from the preparation of Siloxane A1 was mixed with 10.6 g of a tetraethoxysilane hydrolysate oligomer (marketed as "SILIKAT TES 40" by Wacker Chemie AG, Munich, Germany) having a SiO2 content of 40% for total hydrolysis and condensation, 6.3 g of a methyltriethoxysilane hydrolysate oligomer having an average of 10 Si atoms per molecule, and 6.3 g of 3-aminopropyltriethoxysilane, and 12.6 g of the equilibrium product, and the mixture was stirred at 200 revolutions / min for an additional 5 minutes. Subsequently, a surface area of ​​150 m² 244 g of hydrophilic exothermic silica (marketed by Wacker Chemie AG under the name HDK® V15A) was added, and the mixture was stirred at 200 revolutions / min for an additional 5 minutes until all the exothermic silica was wetted. Then, stirring was continued at 600 revolutions / min for 10 minutes under reduced pressure of 200 mbar. Finally, 3 g of a solution of octylphosphonic acid at 33 wt% in phenyltrimethoxysilane and 1.58 g of a solution of 0.27 g of dioctyltin oxide in 1.31 g of an equilibrium product consisting of 0.655 g of methyltriethoxysilane hydrolysate oligomer having an average of 10 Si atoms per molecule and 0.655 g of 3-aminopropyltriethoxysilane were added, and the mixture was stirred under reduced pressure (200 mbar) for an additional 5 minutes.

[0220] Next, the mixture was dispensed into standard commercial cartridges and stored in a moisture-free environment. 24 hours after the mixture was prepared, a 2 mm thick plaque was removed from the mixture, and after curing the plaque at 23°C and 50% relative humidity for 7 days, a Type 2 dumbbell specimen was prepared according to ISO 37, 6th edition 2017-11.

[0221] The results are shown in Table 1.

[0222] Example 2

[0223] Preparation of oligomer mixture B2-2

[0224] 240 g (3.25 mol) of α,ω-bis(trimethylsiloxy)polydimethylsiloxane with a viscosity of 1000 mPas in ethanol, 234 g (1.0 mol) of trimethoxy(2,4,4-trimethylpentyl)silane (=iOctSi(OMe)3) (marketed by Wacker Chemie AG under the name SILRES® BS-1316), and 0.80 g of a sodium ethoxide (21%) solution were mixed, and the mixture was heated at 110°C for 4 hours. After cooling the solution, 1.60 g of a dimethyldichlorosilane (10%) solution in n-heptane was added to neutralize the mixture. This mixture was devolatilized in a rotary evaporator at 120°C under reduced pressure of 50 mbar. The composition of the mixture was determined by 29-Si NMR spectroscopy. The mixture comprises 1.4 wt% iOctSi(OMe)3, 0.4 wt% Me2Si(OMe)2, and 98.2 wt% [iOctSi(OMe)2O 1 / 2 ] 0.08 [iOctSi(OMe)O 2 / 2 ] 0.15 [iOctSiO 3 / 2 ] 0.05 [Me2SiO 2 / 2 ] 0.43 [Me2Si(OMe)O 1 / 2 ] 0.29 It contained an oligomer mixture having an average composition. The molecular weights determined by gel permeation chromatography were 929 g / mol (Mw) and 635 (Mn). The polydispersity (Mw / Mn) was 1.46.

[0225] Preparation of Mixture M2

[0226] The preparation of mixture M1 as described in Example 1 was repeated. Additionally, 36 g of the aforementioned oligomer mixture B2-2 was mixed.

[0227] Mixture M2 was subsequently dispensed into a standard commercial cartridge and stored in a moisture-free environment. 24 hours after the mixture was prepared, a 2 mm thick plaque was removed from the mixture, and after curing the plaque at 23°C and 50% relative humidity for 7 days, a Type 2 dumbbell specimen was prepared according to ISO 37, 6th edition 2017-11.

[0228] The results are shown in Table 1.

[0229] Example 3

[0230] Preparation of Siloxane A3

[0231] A mixture of 660 g of α,ω-dihydroxypolydimethylsiloxane with a viscosity of 80,000 mPas and 220 g of α,ω-dihydroxypolydimethylsiloxane with a viscosity of 20,000 mPas was stirred at 200 revolutions / min for 30 minutes with 30.44 g of a solution of 0.04 g of 1,5,7-triazabicyclo[4.4.0]dex-5-ene in 30.4 g of phenyltrimethyloxysilane. After a reaction time of 30 minutes, a mixture of 98.0 wt% of α,ω-bis((phenyldimethoxysilyl)polydimethylsiloxane) with a viscosity of 51,000 mPas, 1.9 wt% of phenyltrimethoxysilane, and 0.1 wt% of methanol was obtained.

[0232] Preparation of Mixture M3

[0233] The procedure for preparing mixture M1 as described in Example 1 was repeated, but the siloxane used was modified to be siloxane A3 instead of A1.

[0234] Mixture M3 was subsequently dispensed into standard commercial cartridges and stored in a moisture-free environment. 24 hours after the mixture was prepared, a 2 mm thick plaque was removed from the mixture, and after curing the plaque at 23°C and 50% relative humidity for 7 days, a Type 2 dumbbell specimen was prepared according to ISO 37, 6th edition 2017-11.

[0235] The results are shown in Table 1.

[0236] Example 4

[0237] Preparation of Mixture M4

[0238] The procedure for preparing mixture M1 as described in Example 1 was repeated, but the siloxane used was modified to be siloxane A3 instead of A1. Additionally, 36 g of the aforementioned oligomer mixture B2-2 was mixed.

[0239] Mixture M4 was subsequently dispensed into standard commercial cartridges and stored in a moisture-free environment. 24 hours after the mixture was prepared, a 2 mm thick plaque was removed from the mixture, and after curing the plaque at 23°C and 50% relative humidity for 7 days, a Type 2 dumbbell specimen was prepared according to ISO 37, 6th edition 2017-11.

[0240] The results are shown in Table 1.

[0241] Example 5

[0242] Preparation of Siloxane A5

[0243] A mixture of 660 g of α,ω-dihydroxypolydimethylsiloxane with a viscosity of 80,000 mPas and 220 g of α,ω-dihydroxypolydimethylsiloxane with a viscosity of 20,000 mPas was stirred at 200 revolutions / min for 60 minutes with 53.2 g of a solution of 1,5,7-triazabicyclo[4.4.0]dex-5-ene in 0.1 g of n-hexadecyltrimethoxysilane. After a reaction time of 60 minutes, a mixture of 95.3 wt% of α,ω-bis(n-hexadecyldimethoxysilyl)polydimethylsiloxane with a viscosity of 50,200 mPas, 4.6 wt% of n-hexadecyltrimethoxysilane, and 0.1 wt% of methanol was obtained.

[0244] Preparation of Mixture M5

[0245] The procedure for preparing mixture M1 as described in Example 1 was repeated, but the siloxane used was modified to be siloxane A5 instead of A1. Additionally, 36 g of the aforementioned oligomer mixture B2-2 was mixed.

[0246] Mixture M5 was subsequently dispensed into standard commercial cartridges and stored in a moisture-free environment. 24 hours after the mixture was prepared, a 2 mm thick plaque was removed from the mixture, and after curing the plaque at 23°C and 50% relative humidity for 7 days, a Type 2 dumbbell specimen was prepared according to ISO 37, 6th edition 2017-11.

[0247] The results are shown in Table 1.

[0248] Example 6

[0249] Preparation of Siloxane A6

[0250] A mixture of 660 g of α,ω-dihydroxypolydimethylsiloxane with a viscosity of 80,000 mPas and 280 g of α,ω-trimethylsiloxypolydimethylsiloxane with a viscosity of 10 mPas was stirred at 200 rotations / min for 30 minutes with 38.24 g of a solution of 1,5,7-triazabicyclo[4.4.0]dex-5-ene in 0.04 g of phenyltrimethoxysilane in 38.2 g of phenyltrimethoxysilane. After a reaction time of 30 minutes, a mixture of 98.0 wt% of α,ω-bis(phenyldimethoxysilyl)polydimethylsiloxane with a viscosity of 50,800 mPas, 1.9 wt% of phenyltrimethoxysilane, and 0.1 wt% of methanol was obtained.

[0251] Preparation of Mixture M6

[0252] 455 g of the reaction mixture obtained from the preparation of Siloxane A6 was mixed with 11.1 g of the equilibrium product of 5.55 g of a methyltriethoxysilane hydrolysate oligomer having an average of 10 Si atoms per molecule and 5.55 g of 3-aminopropyltriethoxysilane, and the mixture was stirred at 200 revolutions / min for an additional 5 minutes. Subsequently, a surface area of ​​150 m² 242.2 g of hydrophilic exothermic silica (marketed by Wacker Chemie AG under the name HDK® V15A) was added, and the mixture was stirred at 200 revolutions / min for an additional 5 minutes until all the exothermic silica was wetted. Then, stirring was continued at 600 revolutions / min for 10 minutes under reduced pressure of 200 mbar. Finally, 1.78 g of a solution of 0.30 g of dioctyltin oxide was added to 2.2 g of a solution of octylphosphonic acid at 33 wt% in phenyltrimethoxysilane and 1.48 g of an equilibrium product consisting of 0.74 g of methyltriethoxysilane hydrolysate oligomer having an average of 10 Si atoms per molecule and 0.74 g of 3-aminopropyltriethoxysilane, and the mixture was stirred under reduced pressure (200 mbar) for an additional 5 minutes.

[0253] Mixture M6 was subsequently dispensed into a standard commercial cartridge and stored in a moisture-free state. 24 hours after the mixture was prepared, a 2 mm thick plaque was removed from the mixture, and after curing the plaque at 23°C and 50% relative humidity for 7 days, a Type 2 dumbbell specimen was prepared according to ISO 37, 6th edition 2017-11.

[0254] The results are shown in Table 1.

[0255]

[0256] No contamination of the margins was found in any of the examples.

[0257] After wetting the test specimen with water, no hydrophobic regions were found in the sandstone.

Claims

Claim 1 A composition capable of being crosslinkable by a condensation reaction and prepared using the following (A), (B1) and optionally (B2), wherein the composition contains an organosilicon compound having a molecular weight of 195 g / mol or less in an amount of less than 0.5 weight% based on the organopolysiloxane (A): (A) an organopolysiloxane (R) of the following chemical formula (I) 2 O) 3-a SiR 1 a O(SiR2O) n SiR 1 a (OR 2 ) 3-a (I)(wherein R may be the same or different and represents a monovalent, optionally substituted hydrocarbon radical, and R 1 may be the same or different and represents a monovalent, optionally substituted hydrocarbon radical, and R 2 may be the same or different and represents a monovalent, optionally substituted hydrocarbon radical, a may be the same or different and is 0 or 1, n is an integer from 380 to 2000, provided that the viscosity at 25°C is 6000 mPas or higher, and R 1 It is a phenyl radical, radical -CH2-NR 6' R 5' or radical CH2NR 11' and, here R 5' represents a hydrocarbon radical having 1 to 12 carbon atoms, and R 6' is a hydrogen atom or radical R 5' Represents, and R 11' represents a divalent hydrocarbon radical in which a heteroatom may be interposed.)(B1) Silane R of the following chemical formula (II) 3 4-b (R 4 O) b Si (II)(in the formula, R 3 may be the same or different and represents a monovalent, SiC-bonded, optionally substituted hydrocarbon radical, and R 4 (B2) silicon compound R composed of units of the following formula (III) 7 c (R 8 O) d SiO (4-c-d) / 2 (III)(In the formula, R 7 may be the same or different and represents a monovalent, SiC-bonded, optionally substituted hydrocarbon radical, and R 8 may be the same or different and represents a monovalent, optionally substituted hydrocarbon radical, c is 0, 1 or 2, and d is 0, 1, 2 or 3, provided that the sum of c+d in formula (III) is ≤3, and at least two groups (R) in the silicon compound 8 O) is present, and the viscosity at 25℃ is less than 2000 mPas.) Claim 2 In paragraph 1, radical R 3 A composition characterized by being a linear, branched, or cyclic hydrocarbon radical having 1 to 16 carbon atoms, or a monovalent hydrocarbon radical having 1 to 12 carbon atoms substituted with an amino group on a carbon atom bonded to a silicon atom. Claim 3 A composition according to claim 1 or 2, characterized in that component (B1) comprises tetraethoxysilane, 2,2,4-trimethylpentyltrimethoxysilane, (2,3,5,6-tetrahydro-1,4-oxazine-4-yl)methyltriethoxysilane, phenyltrimethoxysilane, or n-hexadecyltrimethoxysilane. Claim 4 A composition according to claim 1 or 2, characterized by including component (B1) in an amount of 0.5 to 7 parts by weight based on 100 parts by weight of component (A). Claim 5 A composition according to claim 1 or 2, characterized by comprising an organosilicon compound having a molecular weight of 195 g / mol or less in an amount of less than 0.1 weight% based on organopolysiloxane (A). Claim 6 A composition according to claim 1 or 2, characterized in that it is a composition that can be prepared using (A) an organopolysiloxane of formula (I), (B1) a silane of formula (II), (B2) a silicon compound consisting of units of formula (III), optionally (C) an adhesion promoter, optionally (D) a curing promoter, optionally (E) a plasticizer, optionally (F) a filler, and optionally (G) an additive. Claim 7 A composition characterized by not containing a plasticizer (E) in claim 1 or 2. Claim 8 A method for preparing the composition claimed in claim 1 by mixing components (A), (B1) and optionally (B2). Claim 9 A molded article manufactured by crosslinking a composition manufactured as claimed in claim 1 or 2, or as claimed in claim 8.

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