Emulsions or organosilicon compounds for waterproofing...

Details Emulsions or organosilicon compounds for waterproofing... Emulsions or organosilicon compounds for waterproofing...

2000-03-16

2001-07-17

Wu, David W. (Department: 1713)

Synthetic resins or natural rubbers -- part of the class 520 ser

Synthetic resins

At least one aryl ring which is part of a fused or bridged...

C524S837000, C106S287110, C106S287130, C106S287160

Reexamination Certificate

active

06262171

ABSTRACT:

The invention relates to aqueous emulsions of organosilicon compounds for waterproofing porous mineral building materials, and also a process for waterproofing the building materials using the emulsions.
Aqueous emulsions of organosilicon compounds are used for protection of buildings primarily because of their excellent impregnation action against water and dirt, their compatibility with the environment and their physiological acceptability.
U.S. Pat. No. 4,757,106 describes the impregnation of neutral mineral building materials with an aqueous emulsion of polvorganosiloxane containing ammonium groups and polyorganosiloxane containing ethoxy groups.
The waterproofing action is lower on alkaline building materials since the ammonium groups are neutralized and the emulsion breaks. The polyorganosiloxanes can then hardly penetrate into the building material. emulsions which contain resinous, alkoxyl-containing polyorganosiloxanes as active ingredients penetrate well into porous building materials and give these good surf ace hydrophobicity. However, dense building materials are protected only on the surface and for a limited time.
Although emulsions of alkylalkoxysilanes do penetrate well into building materials, they are not storage stable. EP-A-340 816 describes buffered emulsions of alkylalkoxysilanes which are storage stable but, particularly in neutral building materials, precipitate too slowly and therefore give poor waterproofing.
Emulsions which contain resinous, alkoxyl-containing polyorcanosiloxanes and a kylalkoxysilanes as active ingredient are known from U.S. Pat. No. 5,091,002. These emulsions are a compromise between storage stability and waterproofing action on the surface.
The previously known emulsions which contain no polyorganosiloxane containing ammonium groups have poor storage stability in diluted form and display an unsatisfactory early water resistance.
It is an object of the invention to provide storage-stable aqueous emulsions of organosilicon compounds for waterproofing porous mineral building materials and coatings for buildings, and also a process for waterproofing porous mineral building materials and coatings for buildings which is particularly effective for neutral and basic building materials and coatings for buildings.
The invention provides an aqueous emulsion comprising the components
(A) organosilicone compositions
(A1) C
1
-C
20
-alkyl-C
2
-C
6
-alkoxysilanes and
(A2) organopolysiloxane containing alkoxy groups,
(B) organopolysiloxane containing, in addition to other organosiloxane units, siloxane units having SiC-bonded radicals containing basic nitrogen, with the proviso that the amine number of the organopolysiloxane is at least 0.01, and
(C) an emulsifier.
Preferably, the C
1
-C
20
-alkyl-C
2
-C
6
-alkoxysilanes (A1) possess 1 or 2 identical or different, unsubstituted or halogen-substituted, SiC-bonded monovalent C
1
-C
20
-alkyl radicals and the remaining radicals are identical or different C
2
-C
6
-alkoxy radicals. Methoxysilanes hydrolyze too quickly and prevent sufficient storage stability.
Examples of the C
1
-C
20
-alkyl radicals are the methyl, ethyl, n-propyl, iso-propyl, n-butyl, iso-butyl, tert-butyl, n-pentyl, iso-pentyl, neo-pentyl, tert-pentyl radical; hexyl radicals such as the n-hexyl radical; heptyl radicals such as the n-heptyl radical; octyl radicals such as the n-octyl radical and iso-octyl radicals such as the 2,2,4-trimethylpentyl radical; nonyl radicals such as the n-nonyl radical; decyl radicals such as the n-decyl radical and dodecyl radicals such as the n-dodecyl radical; cycloalkyl radicals such as the cyclopentyl, cyclohexyl, 4-ethylcyclohexyl, cycloheptyl radicals, norbornyl radicals and methylcyclohexyl radicals.
Examples of halogen-substituted C
1
-C
20
-alkyl radicals are alkyl radicals substituted by fluorine, chlorine, bromine and iodine atoms, for example the 3,3,3-trifluoro-n-propyl radical, the 2,2,2,2′,2′,2′-hexafluoroisopropyl radical and the heptafluoroiso-propyl radical.
Particular preference is given to the unsubstituted C
1
-C
12
-alkyl radicals.
Exampies of C
2
-C
6
-alkoxy radicals are the ethoxy, n-propoxy, iso-propoxy, n-butoxy, iso-butoxy, sec-butoxy, tert-butoxy radical; pentyloxy radicals such as the n-pentyloxy radical and hexyloxy radicals such as the n-hexyloxy radical. The ethoxy radicals are particularly preferred.
The alkoxy radicals can be substituted by halogen atoms, but this is not preferred.
The emulsion can contain one organopolysiloxane containing alkoxy groups (A2) or a mixture of a plurality of organopolysiloxanes. The organopoly-siloxanes can additionally contain hydroxyl groups which aid binding to the building materials.
The organopolysiloxanes (A2) preferably have a viscosity of at most 2000 mm
2
/s so as to achieve a particularly good distribution on the pore surfaces in the masonry.
Particular preference is given to the organopolysiloxanes (A2) comprising units of the general formula (I)
R
x
⁢
Si
⁡
(
O
⁢
R
1
)
y
⁢
(
OH
)
z
⁢
O
4
-
x
-
y
-
z
2
(
I
)
where
R are identical or different monovalent, unsubstituted or halogen-substituted, SiC-bonded C
1
-C
20
-hydrocarbon radicals,
R
1
are identical or different monovalent, C
1
-C
6
-alkyl radicals,
x is 0, 1, 2 or 3, on average from 0.8 to 1.8,
y is 0, 1, 2 or 3, on average from 0.01 to 2.0 and
z is 0, 1, 2 or 3, on average from 0.0 to 0.5, with the proviso that the sum of x, y and z is at most 3.5.
The organopolysiloxane (A2) preferably has a viscosity of from 10 mm
2
/s to 50,000 mm
2
/s, in particular from 50 mm
2
/s to 5000 mm
2
/s, at 25° C.
Examples of the C
1
-C
20
-hydrocarbon radicals are the C
1
-C
20
-alkyl radicals and halogen-substituted C
1
-C
20
-alkyl radicals listed above for the organalkoxysilanes (A1), alkenyl radicals such as the vinyl, allyl, n-5-hexenyl, 4-vinylcyclohexyl and 3-norbornenyl radical; aryl radicals such as the phenyl, biphenylyl, naphthyl, anthryl and phenanthryl radical; alkaryl radicals such as the o-, m-, p-tolyl radicals, xylyl radicals and ethylphenyl radicals; aralkyl radicals such as the benzyl radical, the alpha- and the &bgr;-phenylethyl radical. Particular preference is given to the unsubstituted C
1
-C
12
-alkyl radicals and the phenyl radical.
Although not indicated in the above formula, part of the radicals R can be replaced by hydrogen atoms directly bonded to silicon atoms. However, this is not preferred.
Examples of the radicals R
1
are the methyl, ethyl, n-propyl, iso-propyl, n-butyl, sec-butyl and tert-butyl radical; pentyl radicals such as the n-pentyl radical and hexyl radicals such as the n-hexyl radical, with the ethyl radical being particuarly preferred.
x preferably has an average value of from 0.9 to 1.1. y preferably has an average value of from 0.4 to 1.2. z preferably has an average value of from 0.0 to 0.2.
Examples of organosiloxanes (A2) are those which are obtainable by reaction of methyltrichlorosilane and, if desired, a C
1
-C
8
-alkyltrichlorosilane, or phenyltrichlorosilane with ethanol in water, such as the organopolysiloxanes of the empirical formulae
CH
3
Si (OC
2
H
5
)
0.8
O
1.1
or
C
6
H
5
Si (OC
2
H
5
)0.72O
1.14
.
The organopolysiloxanes (B) are preferably ones comprising units of the general formula (II)
R
a
2
⁢
R
b
3
⁡
(
O
⁢
R
4
)
c
⁢
SiO
4
-
a
-
b
-
c
2
,
(
II
)
where
R
2
are identical or different monovalent, unsubstituted or halogen-substituted, SiC-bonded C
1
-C
20
-hydrocarbon radicals which are free of basic nitrogen,
R
3
are identical or different monovalent, unsubstituted or halogen-substituted, SiC-bonded C
1
-C
30
-hydrocarbon radicals containing basic nitrogen,
R
4
can be identical or different and can be hydrogen atoms or C
1
-C
6
-alkyl radicals,
a is 0, 1, 2 or 3,
b is 0, 1, 2 or 3, on average at least 0.05, and
c is 0, 1, 2 or 3,
with the proviso that the sum of a, b and c is less than or equal to 3 and the amine number of the organopolysiloxane (B) is at least 0.01.
The amine number is the number of ml of 1N HCl which are recuired for neutralization of 1 g of organopolysil

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