Colloid systems and wetting agents; subcombinations thereof; pro – Compositions containing a wetting agent; processes of... – The agent contains organic compound containing phosphorus
Reexamination Certificate
1999-06-22
2003-04-08
Sergent, Rabon (Department: 1711)
Colloid systems and wetting agents; subcombinations thereof; pro
Compositions containing a wetting agent; processes of...
The agent contains organic compound containing phosphorus
C252S182240, C252S182300, C516S031000, C516S033000, C516S034000, C524S418000, C524S424000, C524S425000, C524S430000, C524S433000, C524S436000, C524S442000, C524S443000, C524S445000, C524S449000
Reexamination Certificate
active
06545059
ABSTRACT:
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to a method for the treatment of mineral fillers using organic phosphate treatment agents.
The invention also relates to the mineral fillers so treated and that can be suspended in a polyol.
The invention also relates to such suspensions of these treated mineral fillers in polyols, as well as to their use in the manufacture of flexible, semirigid, or rigid polyurethane foams.
Finally, the invention relates to the use of flexible, semirigid, or rigid polyurethane foams containing these treated mineral fillers in the manufacture of molded or nonmolded objects.
2. Description of the Prior Art
To decrease the cost price per liter and per kilogram of molded or nonmolded objects made from flexible, semirigid, or rigid polyurethane foams, it has been increasingly necessary to increase the quantity of filler present in the flexible, semirigid, or rigid polyurethane foams while at the same time preserving or improving their physicochemical properties, such as, compression, or their aesthetic or other properties, such as fire retardation, which are desired in various fields of industry such as, notably, transports (for example, cars and furniture) and in construction or other fields.
Several methods exist today to introduce mineral fillers, such as calcium carbonate, into these polyurethane compounds.
In a first type of method (French Patent No. 2,651,238), calcium carbonate is introduced into a plasticizer for polyurethane. However, this method for obtaining a suspension of a filler in a plasticizer, which permits increasing the content of the filler in the polyurethane compound, is not suitable for the following reasons. Its cost is high and its use is excessively difficult in the manufacture of flexible, semirigid, or rigid polyurethane foams. In addition, the physicochemical properties of the foams obtained from such suspensions are degraded.
Applicants have invented a method which completely favors the introduction of mineral fillers into flexible, semirigid, or rigid polyurethane foams using an inexpensive, simple means that does not result in any problems involving a significant decrease in the reactivity of the polyurethane foams.
Applicants' method is an improvement over other methods for the introduction of the filler into the polyol, one of the constituents of the polyurethane, that are known to a person skilled in the art.
A first type of method discloses grafting of methacrylic acid (German Patent Nos. 2,654,746, 2,714,291, and 2,739,620) or of another vinyl compound such as styrene on the polyol. However, this type of method does not allow the use of a suspension of calcium carbonate in the polyol because the suspension is too difficult to handle as a result of an excessively high viscosity and a poor distribution of the filler in the medium.
Another type of method involves treating the filler at the surface prior to its introduction into the polyol by means of an agent that is, for example, an alcohol with 8-14 carbon atoms (French Patent No. 2,531,971) or a hydroxycarboxylic acid phosphate (European Patent No. 0,202,394).
However, these methods produce the same type of drawbacks as those cited above since the user is confronted with problems of poor dispersibility—in the polyol—of the mineral filler so treated.
Thus, the techniques heretofore known do not solve the problem of suspending mineral fillers in the polyol, which mineral fillers are intended to be used in the manufacture of flexible, semirigid, or rigid polyurethane foams.
SUMMARY OF THE INVENTION
In order to solve this problem, the applicant developed a method for the treatment of a mineral filler by means of at least one organic phosphate treatment agent, as well as a mineral filler so treated that allows, in an unexpected manner, for the production of a suspension of a mineral filler in polyols with a high content of the filler and a low viscosity; that is, a homogeneous suspension not subject to serious sedimentation, decanting, or thickening in the manufacture of flexible, semirigid, or rigid polyurethane foams.
Thus, one of the objectives of the invention is the development of a method for the treatment of mineral fillers for use in a suspension in polyols, using at least one treatment agent of the organic phosphate type with the general formula (I):
with R
1
=H, C
8
-C
40
alkyl, or C
6
-C
40
aryl, alkylaryl, or arylalkyl radical,
with R
2
=C
8
-C
40
alkyl or C
6
-C
40
aryl, alkylaryl, or arylalkyl radical
(m+n) varies from 0 to 30 with m≦30 and n≦30
(p+q) varies from 0 to 30 with p≦30 and q≦30
Another objective of the invention is the development of these treated mineral fillers which exhibit an uptake of polyol which is decreased by at least 15%, preferably at least 20%, with respect to uptake of polyol using the untreated mineral filler, while at the same time preserving the hydrophilicity of the untreated mineral fillers.
Another objective of the invention is the development of homogeneous, stable, and low-viscosity suspensions of these treated mineral fillers in the polyols, characterized by a concentration by weight of mineral fillers that can be up to 80% and a treatment agent content up to 0.5-3 wt % based on the dry weight of the filler.
These homogeneous, stable, and low-viscosity suspensions according to the invention can easily be handled because, under normal conditions of use, they present no decanting phenomenon, that is, no separation into two phases; no sedimentation, that is, no presence of a hard deposit at the bottom of the vessel in which the suspension is stored; and no serious thickening, thus allowing for the production of flexible, semirigid, or rigid polyurethane foams with excellent physicochemical properties.
Finally, another objective of the invention is the use of these homogeneous, stable, and low-viscosity suspensions of mineral fillers in the manufacture of flexible, semirigid, or rigid polyurethane foams as well as the use of said foams in the manufacture of molded or nonmolded objects.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
These objectives are attained by a preferred treatment method according to which at least one treatment agent with the general formula (I) is mixed with the mineral filler to be treated so as to obtain a homogeneity factor (HF) of less than 0.2, preferably less than 0.10, and very preferably less than 0.05, with said factor being defined as the difference in weight between the retained material during dry sieving of the treated fillers and the retained material during dry sieving of nontreated fillers, which is expressed by the formula:
HF
=
(
weight
of
the
treated
filler
that
remained
on
the
sieve
)
(
weight
of
the
test
sample
of
the
treated
filler
)
-
(
weight
of
the
nontreated
filler
that
remained
on
the
sieve
)
(
weight
of
the
test
sample
of
the
nontreated
filler
)
and measured by the use of a sieve according to the standard NF Xll-501 (325 mesh size). (This standard is publicly available at AFNOR, the French organization of standards.)
This method for measuring the retained quantity during dry sieving involves weighing very precisely 100 g of the filler test sample, followed by pouring the sample into the sieve with a size of 325 mesh.
The sieve is then placed on a mechanical sieve marketed by the company RETSCH GmbH as type 3D and driven, for 30 min, in an oscillatory motion corresponding to a graduation from 50 to 100. After 30 min, the dry retained quantity remaining on the sieve is subjected to the moderate action of a brush in accord
Blanchard Pierre
Fichou Jean-Pierre
Husson Maurice
Ravet Georges
Oblon & Spivak, McClelland, Maier & Neustadt P.C.
Omya S.A.
Sergent Rabon
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