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Patent 2057110 Summary

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(12) Patent: (11) CA 2057110
(54) English Title: WATER-CONTAINING ORGANOPHILIC PHYLLOSILICATES
(54) French Title: PHYLLOSILICATES ORGANOPHILES RENFERMANT DE L'EAU
Status: Deemed expired
Bibliographic Data
(51) International Patent Classification (IPC):
  • C09D 1/00 (2006.01)
  • D21H 19/40 (2006.01)
  • D21H 19/46 (2006.01)
(72) Inventors :
  • DESSAUER, GUIDO (Germany)
  • HORN, UTE (Germany)
(73) Owners :
  • BRABON GMBH & CO. KG (Germany)
(71) Applicants :
(74) Agent: FETHERSTONHAUGH & CO.
(74) Associate agent:
(45) Issued: 2001-04-10
(22) Filed Date: 1991-12-05
(41) Open to Public Inspection: 1992-06-07
Examination requested: 1997-10-29
Availability of licence: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data:
Application No. Country/Territory Date
P 40 38 886.7 Germany 1990-12-06

Abstracts

English Abstract




The invention relates to the use of water-containing
organophilic phyllosilicates obtained by the reaction of
a phyllosilicate, which is completely delaminated
colloidally in water and is capable of cation exchange,
with an organic onium salt in aqueous suspension and
subsequent mechanical removal of the water, without
drying by heating, as a rheological additive in organic
media.
The water-containing organophilic phyllosilicates are
particularly suitable for coating paper.


Claims

Note: Claims are shown in the official language in which they were submitted.




7
CLAIMS:
1. The use of a water-containing organophilic
phyllosilicate obtained by the reaction of a phyllosilicate,
which is completely delaminated colloidally in water and is
capable of cation exchange, with an organic onium salt in
aqueous suspension and subsequent mechanical removal of the
water, without drying by heating, as a rheological additive in
organic media.
2. The use of a water-containing organophilic
phyllosilicate obtained as claimed in claim 1 for coating paper
from a suspension in an organic solvent.
3. The use as claimed in claim 1 or 2, wherein the
phyllosilicate used for the reaction with the onium salt is a
Na bentonite.
4. The use as claimed in claim 1, wherein the organic
onium salt is an organic quaternary ammonium salt.
5. The use as claimed in claim 1 or 2, wherein the onium
salt is distearyl-dimethyl-ammonium chloride.
6. An organic medium containing a water-containing
organophilic phyllosilicate obtained by the reaction of a
phyllosilicate, which is completely delaminated coloidally in
water and is capable of canon exchange, with an organic onium
salt in aqueous suspension and subsequent mechanical removal of
the water without drying by heating.
7. The organic medium of claim 6 for use in coating
paper from a suspension in an organic solvent.
8. The organic medium of claim 6 or 7 wherein the
phyllosilicate used for the reaction with the onium salt is a
Na bentonite.



8
9. The organic medium of claim 6, 7 or 8 wherein the
organic onium salt is an organic quaternary ammonium salt.
10. The organic medium of any one of claims 6 to 9
wherein the onium salt is distearyl-dimethyl-ammonium chloride.
11. A method of preparing an organic medium containing a
water-containing organophilic phyllosilicate comprising the
steps of:
a) preparing a water-containing organophilic
phyllosilicate obtained by the reaction of a
phyllosilicate which is completely delaminated
colloidally in water and is capable of cation
exchange, with an organic onium salt in aqueous
suspension and subsequent mechanical removal of
the water without drying by heating; and
b) adding the water-containing organophilic
phyllosilicate of step a) to an organic medium.

Description

Note: Descriptions are shown in the official language in which they were submitted.





20~'~l.~.r
HOECHST ARTIEPIGESELLSCHAFT HOE 90/F 364 Dr.ICI/1
Description
Water-containing organophilic phyllosilicates
It is widely known that organophilically modified
phyllosilicates can be employed as Theological additives
in organic media. Examples of these are the commercial
products marketed under the names ~Tixogel (manufacturer:
Sudchemie AG) and ~Bentone. These theological additives
have the effect of the build-up of a thixotropic struc- '
tuts in organic media, for example in paints and var-
nishes. As a result of this thixotropic structure, such
organic media are easier to process . The organophilically
modified phyllosilicates are obtained by treating phyllo-
silicates in aqueous suspension with an aqueous solution
of an onium compound, preferably a quaternary organic
ammonium salt, this organic ammonium salt being embedded
between the layers of the phyllosilicate. The phyllo-
silicate organophilically modified in this manner is then
separated from the water by filtration and dried under
the action of heat, for example in a drum drier at about
100°C. The modified organophilic phyllosilicates obtained
in this manner are water-insoluble.
Such a drying operation has previously been considered
necessary, since the filtercake obtained when the water
is filtered off contains considerable amounts of water,
and this water content has been said to interfere in the
use of the organophilic phyllosilicates in the organic
media. It has now been found, surprisingly, that this is
not the case and that the filtercake of such organophilic
phyllosilicates can be employed as a Theological additive
in organic media even without being dried.
The invention thus relates to the use of water-containing
organophilic phyllosilicates which are obtained by the
reaction of a phyllosilicate, which is completely
delaminated colloidally in water and is capable of ration
exchange, with an organic onium salt in aqueous




- 2 -
suspension and subsequent mechanical removal of the
water, without drying by heating, as a rheological
additive in organic media and for coating paper.
These organophilic phyllosilicates are obtained by
methods which are known per se, which therefore do not
have to be explained in more detail. Possible phyllo-
silicates which are capable of cation exchange and are
completely delaminated colloidally in water are all the
synthetic or naturally occurring smectic phyllosilicates,
preferably bentonite or montmorillonite, which, in
addition to a smectic phyllosilicate, can also contain
25-30~ by weight of impurities in the form of other
minerals. The minerals are treated with an aqueous
solution of onium compounds, such as, for example,
phosphonium compounds, but preferably quaternary organic
ammonium salts, these compounds being embedded between
the layers of these minerals. Possible quaternary organic
ammonium salts are, in particular, compounds of the
formula
R, Rz
2 0 ~ N ~ A°'
R,/ ~Rz
in which Rl is C8-CZZ-alkyl or C8-CZZ-alkenyl, RZ is Cl-Cd-
alkyl and A is an anion, preferably chloride or metho-
sulfate. The compound distearyl-dimethyl-ammonium
chloride is particularly preferred. When the phyllo-
silicate is charged with the quaternary organic ammonium
salt, the water is filtered off or pressed off. This is
done by the customary processes of separation. The
filtercake obtained consists, depending on the purity of
the phyllosilicates, to the extent of about 65 to 83$ of
water and is employed according to the invention in this
form directly as a rheological additive in organic media.
Examples of organic media in the sense of this invention



- 3 -
are paints, varnishes, coatings, putties, lubricating
greases, cosmetics, paint removers, filler compositions
and similar formulations containing organic solvents. The
water-containing organophilically modified phyllo-
silicates according to the invention have a thixotroping
effect in all these systems. As a result of this effect, .
the formulations mentioned are easier to process. In
addition, these phyllosilicates also prevent settling of
the insoluble components, for example the pigments within
these media. As another surprising effect of these water
containing organophilic phyllosilicates it has been found
that the thickening action here is significantly higher
in comparison with the analogous commercially available
products having the same solids content, but from which
the water has been removed by drying by heating.
These water-containing organophilically modified phyllo-
silicates are added to the organic media by methods which
are known per se. The amount of these rheological addi-
tives also lies within the range known to the expert in
this field (about 0.5 to 3% by weight).
The water-containing organophilic phyllosilicates accord-
ing to the invention are particularly suitable for
coating paper. From economic considerations, efforts are
made to use thin printing papers for printed products
with a high circulation, for example newspapers or mail-
order catalogs. However, problems arise here in respect
of opacity, i.e. in the case of printing the print shows
through in an interfering manner on the other side of the
paper. To prevent this effect, it is already known
(EP 192 252) that paper can be coated with an organo-
philic complex of a smectic phyllosilicate and a
quaternary organic ammonium compound from a suspension in
organic solvents. The starting material is present here
in a form from which as much of the water as possible has
been removed by heating. In the context of the present
invention, it has now been found that drying of the
organophilically modified phyllosilicate can be dispensed


- 4 -
with in this process (solvent coating) and the water-
containing presscake of this organophilically modified
phyllosilicate can be employed directly. It is surprising
here that the water in the presscake does not interfere
with the homogeneity of the overall organic system. The
water remains in the inner phase, and no swelling of the
paper fibers occurs, as would be the case with an aqueous
coating. This finding is therefore of relatively great
importance, since in future such "solvent coating"
processes based on toluene or white spirit will gain
increasing importance. The solids content (i.e. without
the content of water from the presscake) of such suspen-
sions is about 3 to 9% by weight. These "solvent coating"
suspensions can furthermore also contain white pigments
(TiOz). As a result of the ability of the organo-
philically modified phyllosilicates to form films, these
white pigments are bonded firmly to the paper by the
phyllosilicates; no additional binder is therefore
needed. A good hold-out effect is obtained in this
manner, i.e. print-through on the printed paper is
prevented.
Examples
A commercially available, non-purified Na bentonite
(exchange capacity 80 milliequivalents/100 g) was stirred
in a hot solution of distearyl-dimethyl-ammonium chloride
at a ratio of the two products of 69% by weight of Na
bentonite and 31% by weight of quaternary organic
ammonium salt. When the reaction had ended, the mixture
was filtered and the now organophilically modified
bentonite was pressed off to a solids content of about
31% by weight. This filtercake was dispersed in toluene
and the dispersion was applied in a thin layer to a sheet
of paper and dried. The details of the examples and the
particular evaluation of the hold-out effect can be seen
from the following Tables 1 and 2.
As the examples show, a very good hold-out effect is



- 5 -
obtained with the water-containing organophilic
phyllosilicates according to the present invention. The
examples in the table show that customary white pigments
can also be applied to the paper and firmly anchored
there by means of the dispersion of the organophilically
modified phyllosilicate in toluene; no additional binder
is required here.
Table 1
1 2 3


Toluene 87.5 g 85 g 82.5 g


Filtercake 12.5 g 15 g 17.5 g


Brookfield viscosity


in mPas at 100
rpm


after 2 days 308 528 720


Weight applied 1.5-1.8 1.6-1.7 1.4-1.6


(g/m2)


Hold-out good good good


Weight applied


(g/mz) 2.3-2.5 2.8-3.0 2.5-2.7


Hold-out very goo best very good





- 6 -
Table 2
3 4 5


Toluene to 100 to 100 to 100


Filtercake 15 g 15 g 15 g


Titanium dioxide 0.4 g



China clay 0.4 g


Optical 0.1 g


brightener



Brookfield viscosity


in mPas at 100 rpm


after 2 days 29g 324 216


Weight applied


g/mz~ 1.3 1.4 1.5


Hold-out good good good



Representative Drawing

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Administrative Status

For a clearer understanding of the status of the application/patent presented on this page, the site Disclaimer , as well as the definitions for Patent , Administrative Status , Maintenance Fee  and Payment History  should be consulted.

Administrative Status

Title Date
Forecasted Issue Date 2001-04-10
(22) Filed 1991-12-05
(41) Open to Public Inspection 1992-06-07
Examination Requested 1997-10-29
(45) Issued 2001-04-10
Deemed Expired 2002-12-05

Abandonment History

There is no abandonment history.

Payment History

Fee Type Anniversary Year Due Date Amount Paid Paid Date
Registration of a document - section 124 $100.00 1991-12-05
Application Fee $0.00 1991-12-05
Maintenance Fee - Application - New Act 2 1993-12-06 $100.00 1993-11-29
Maintenance Fee - Application - New Act 3 1994-12-05 $100.00 1994-12-01
Maintenance Fee - Application - New Act 4 1995-12-05 $100.00 1995-11-27
Maintenance Fee - Application - New Act 5 1996-12-05 $150.00 1996-11-27
Registration of a document - section 124 $100.00 1997-10-22
Maintenance Fee - Application - New Act 6 1997-12-05 $150.00 1997-10-24
Request for Examination $400.00 1997-10-29
Maintenance Fee - Application - New Act 7 1998-12-07 $150.00 1998-09-30
Maintenance Fee - Application - New Act 8 1999-12-06 $75.00 1999-11-22
Maintenance Fee - Application - New Act 9 2000-12-05 $75.00 2000-12-01
Final Fee $150.00 2001-01-05
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
BRABON GMBH & CO. KG
Past Owners on Record
DESSAUER, GUIDO
HOECHST AKTIENGESELLSCHAFT
HORN, UTE
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Abstract 1994-04-01 1 16
Claims 2000-08-16 2 64
Cover Page 2001-03-23 1 23
Claims 1994-04-01 1 41
Description 1994-04-01 6 233
Cover Page 1994-04-01 1 16
Correspondence 2000-12-01 1 23
Correspondence 1999-12-20 3 82
Prosecution-Amendment 2000-02-16 2 5
Fees 1998-09-30 1 42
Prosecution-Amendment 2000-08-16 4 128
Fees 2000-12-01 1 40
Correspondence 2001-01-05 2 53
Prosecution-Amendment 1998-06-26 4 141
Assignment 1991-12-05 5 142
Prosecution-Amendment 1997-10-29 1 40
Fees 1996-11-27 1 196
Fees 1995-11-27 1 184
Fees 1994-12-01 1 196
Fees 1993-11-29 1 151