Gel compositions based on reaction products of polyols and...

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...

Reexamination Certificate

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C524S492000, C524S497000

Reexamination Certificate

active

06809143

ABSTRACT:

INTRODUCTION AND BACKGROUND
The present invention relates to gel compositions based on reaction products of polyols and polyisocyanates.
Gel compositions based on reaction products of polyols and polyisocyanates (polyurethanes)are used in pressure distributing elements, for example in cushions for wheelchairs (EP 0 511 570 B1). The known gel compositions may contain inorganic fillers, such as for example barytes, chalk, gypsum, kieserite, sodium carbonate, titanium dioxide, quartz sand, kaolin, carbon black or glass beads.
The known gel compositions have the disadvantage that their mechanical properties, such as for example their mechanical strength and elongation at break, are not adequate.
SUMMARY OF INVENTION
The present invention provides gel compositions based on reaction products of polyols and polyisocyanates, wherein they contain at least one pyrogenically produced oxide of a metal or metalloid as filler.
The pyrogenically produced oxides may preferably be prepared by flame hydrolysis.
Pyrogenically produced oxides of metals and/or metalloids are known from Ullmanns Enzyklopadie der technischen Chemie 4
th
Edition, Vol. 21, pp. 464 (1982).
DETAILED DESCRIPTION OF INVENTION
In one embodiment of the invention the gel compositions may contain physical mixtures of pyrogenically produced oxides of metals and/or metalloids.
The gel compositions according to the invention may also contain pyrogenically produced mixed oxides of metals and/or metalloids.
The following pyrogenically produced oxides may for example be used according to the invention:
silicone dioxide, aluminum oxide, mixed oxide of silicon dioxide and aluminum oxide, titanium dioxide, mixed oxide of titanium dioxide and iron oxide.
According to the invention there may also be used pyrogenically produced oxides that have undergone a surface treatment, such as for example:
Aerosil R 8200, Aerosil R972, Aerosil R974, Aerosil R805
Aerosil R 202, Aerosil R812. These oxides are described in Pigments Leaflet No. 27 (August 1993) published by Degussa AG.
The following may be used as surface-treatment agents:
dimethyl dichlorosilane, trimethyl dichlorosilane, hexamethyl disilazane, polydimethyl siloxanes, and alkyl silanes such as for example trimethoxyoctyl silane.
In particular the following pyrogenically produced oxides may be used:
AERO-
AERO-
AERO-
AERO-
SIL
AEROSIL
AEROSIL
AEROSIL
AEROSIL
AEROSIL
SIL OX
AEROSIL
SIL
AEROSIL
SIL
Test method
90
130
150
200
300
380
50
TT 600
MOX 80
MOX 170
COK 84
Behavior to water
hydrophilic
hydrophilic
Appearance
loose white powder
loose white powder
Surface according
m2/g
90 + 15
130 + 25
150 + 15
200 + 25
300 + 30
380 + 30
50 + 15
200 + 50
80 + 20
170 + 30
170 +
to BET
1)
30
Mean size of the
nm
20
16
14
12
7
7
40
40
30
15

primary particles
Tamped density
g/l
80
50
50
50
50
50
130
60
60
50
50
(approx. value)
2)
Compacted
g/l
120
120
120
120
120
130
product
(additive “V”)
VV product
g/l
50/75
50/75
50/75
(additive “VV”)
g/l
120/150
120/150
Drying loss
3)
%
<1.0
<1.5
<0.59)
<1.5
<1.5
<2.0
<1.5
<2.5
<1.5
<1.5
<1.5
(2 hours at
105° C.) on
leaving the
supplier
Annealing loss
4) 7)
%
<1
<1
<1
<1
<2
<2.5
<1
<2.5
<1
<1
<1
(2 hours at
1000° C.)
pH value
5)
3.7-4.7
3.7-4.7
3.7-4.7
3.7-4.7
3.7-4.7
3.7-4.7
3.8-4.8
3.6-4.5
3.6-4.5
3.6-4.5
3.6-4.3
SiO
2
8)
%
>99.8
>99.8
>99.8
>99.8
>99.8
>99.8
>99.8
>99.8
>98.3
>98.3
82-86
AlO
2
O
3
8)
%
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.08
<0.05
0.3-1.3
0.3-1.3
14-18
Fe
2
O
3
%
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.01
<0.003
<0.01
<0.01
<0.1
TiO
2
8)
%
<0.03
<0.03
<0.03
<0.03
<0.03
<0.03
<0.03
<0.03
<0.03
<0.03
<0.03
HCl
8) 10)
%
<0.025
<0.025
<0.025
<0.025
<0.025
<0.025
<0.025
<0.025
<0.025
<0.025
<0.1
Sieve residue
6)
%
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.2
<0.05
<0.1
<0.1
<0.1
according to
Mocker, 45 mm)
1)
in accordance with DIN 66131
2)
in accordance with DIN ISO 787/XI, JIS K 5101/18 (not sieved)
3)
in accordance with DIN ISO 787/II, ASTM D 280, JIS K 5101/21
4)
in accordance with DIN 55921, ASTM D 1280, JIS K 5101/23
5)
in accordance with DIN ISO 787/IX, ASTM D 1208, JIS K 5101/24
6)
in accordance with DIN ISO 787/XVIII, JIS K 5101/20
7)
referred to the substance dried for 2 hours at 105° C.
8)
referred to the substance annealed for 2 hours at 1000° C.
9)
special anti-moisture packaging
10)
HCl content is part of the annealing loss
11)
V product supplied in 20 kg sacks
12)
VV product is currently supplied exclusively from the Rheinfelden works
AEROSIL
AEROSIL
AEROSIL
AEROSIL
AEROSIL
AEROSIL
AEROSIL
AEROSIL
Test method
R 972
R 974
R 202
R 805
R 812
R 812 S
R 104
R 106
Behavior to water
hydrophobic
Appearance
loose white powder
Surface according to BET
1)
m2/g
110 + 20
170 + 20
100 + 20
150 + 25
260 + 30
220 + 25
150 + 25
250 + 30
Mean size of the primary
nm
16
12
14
12
7
7
12
7
particles
Tamped density/approx. value)
2)
Normal product
g/l
50
50
50
50
50
50
50
50
Compacted product (additive “V”)
g/l
90
90
Drying loss
3)
%
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5


(2 hours at 105° C.) on
leaving the supplier
Annealing loss
4) 7)
%
<2
<2
4-6
5-7
1.0-2.5
1.5-3.0


(2 hours at 1000° C.)
C content
%
0.6-1.2
0.7-1.3
3.5-5.0
4.5-6.5
2.0-3.0
3.0-4.0
1-2
1.5-3.0
pH value
5)
%
3.6-4.4
3.7-4.7
4-6
3.5-5.5
5.5-7.5
5.5-7.5
>4.0
>3.7
SiO
2
8)
%
>99.8
>99.8
>99.8
>99.8
>99.8
>99.8
>99.8
>99.8
AlO
2
O
3
8)
%
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.08
<0.05
Fe
2
O
3
8)
%
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
TiO
2
8)
%
<0.03
<0.03
<0.03
<0.03
<0.03
<0.03
<0.03
<0.03
HCl
8) 10)
%
<0.05
<0.1
<0.025
<0.025
<0.025
<0.025
<0.002
<0.025
1)
in accordance with DIN 66131
2)
in accordance with DIN ISO 787/XI, JIS K 5101/18 (not sieved)
3)
in accordance with DIN ISO 787/II, ASTM D 280, JIS K 5101/21
4)
in accordance with DIN 55921, ASTM D 1280, JIS K 5101/23
5)
in accordance with DIN ISO 787/IX, ASTM D 1208, JIS K 5101/24
6)
referred co substance dried for 2 hours at 105° C.
7)
referred to substance annealed for 2 hours at 1000° C.
8)
special anti-moisture packaging
9)
HCl content is part of the annealing loss
10)
in water: methanol = 1:1
11)
HCl content is part of the annealing loss
12)
V product supplied in 15 kg net sacks
AEROSIL
Properties
R 8200
Behavior to water
hydrophobic
Surface according to BET
m
2
/g
160 ± 25
Tamped density
g/l
ca. 140
Drying loss (2 hrs. at 105° C.)
%
≦0.5
PH value (4% in water)
≧5.5
Carbon content
%
2.0-4.0
SiO
2
%
≧99.8
Fe
2
O
3
%
≦0.01
TiO
2
%
≦0.03
HCl
%
≦0.025
Gel compositions that may be used according to the invention based on reaction products of polyols and polyisocyanates (polyurethanes)are known.
Thus, for example, documents EP 0 511 570 B1, EP 0 057 838 and EP 0 057 839 B1 describe gel compositions that may be used to produce the gel compositions according to the invention.
The present invention also provides a process for the production of the gel compositions according to the invention based on reaction products of polyols and polyisocyanates, wherein a mixture of
a) one or more polyisocyanates and
b) one or more polyol components and
c) at least one pyrogenically produced oxide of a metal or metalloid
is allowed to gel.
The process according to the invention for producing the gel compositions according to the invention may be characterized by the fact that the isocyanate functionality and the functionality of the polyol component is at least 5.2, preferably at least 6.5, and in particular at least 7.5.
The polyol component may comprise a mixture of
a) one or more polyols with hydroxyl numbers of less than 112 and
b) one or more polyols with hydroxyl numbers in the range from 112

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