Hydrophobic precipitated silica

Details Hydrophobic precipitated silica Hydrophobic precipitated silica

1999-06-25

2001-03-06

Lovering, Richard D. (Department: 1712)

Coating processes

Applying superposed diverse coating or coating a coated base

Metallic compound-containing coating

C428S405000, C516S117000

Reexamination Certificate

active

06197384

ABSTRACT:

INTRODUCTION AND BACKGROUND
The present invention relates to a hydrophobic precipitated silica, to a process for the production thereof and to the use thereof.
It is known to hydrophobize precipitated silicas, wherein a wide variety of hydrophobizing agents may be used such as those described in the following: U.S. Pat. No. 3,567,680, DE-AS 24 35 860, GB-A 2 001 303, German patent 15 67 449, DE-AS 11 72 245, DE-B 25 13 608, DE-B 10 74 559, DE-B 12 29 504, EP-A 0 658 523. Thus, the term “hydrophobizing agent” with respect to silica technology is well understood as to its scope and meaning.
Known processes have the disadvantage that two or more stages must sometimes be used, during which the hydrophilic precipitated silica must first be dried and then is not reacted with the silane until a subsequent heat treatment stage; either that or very long reaction times are required despite elevated temperatures.
Moreover, if uniform hydrophobization of the precipitated silica is to be achieved, the precipitated silica must be homogeneously mixed with the silane. However, homogeneous mixing is not possible when an aqueous precipitated silica suspension is used because it is not possible to achieve a homogeneous distribution of the silane due to its hydrophobic properties.
It is therefore an object of the present invention to provide a hydrophobic precipitated silica which does not exhibit these disadvantages.
SUMMARY OF THE INVENTION
The above and other objects can be achieved according to the present invention which provides a hydrophobic precipitated silica which is characterized by the following physical/chemical parameters:
Drying loass
[%]
2.0-10 
DIN ISO 787/2
Ignition loss
[%]
 2-25
DIN ISO 3262/11
Methanol wettability
[%]
20-80
titrated
Carbon content
[%]
 1-30
—
The present invention also provides a process for the production of the hydrophobic precipitated silica, which process is characterized in that an aqueous precipitated silica suspension is produced and is mixed with an aqueous silane emulsion and this mixture is then dried.
The mixture may be produced in batches. In another embodiment of the invention, once the precipitated silica emulsion and the silane emulsion have passed through a mixing section, they can simultaneously be fed into a spray dryer.
In a preferred embodiment of the invention, the mixture can be dried by means of a spray dryer.
Another option for performing mixing and drying is drying by means of a spin/flash dryer.
DETAILED DESCRIPTION OF INVENTION
The present invention will now be described in further detail. Any known precipitated silica may be used as the precipitated silica for purposes of this invention. Such precipitated silicas and the production thereof are described, for example, in Winnacker-Küchler,
Chemische Technologie,
volume 3, 4th edition, page 82 (1983) and in
Ullmanns Encyklopädie der technischen Chemie,
volume 21, 4th edition (1982), pages 465 et seq.
In a preferred embodiment, VN3 may be used as the precipitated silica. VN3 is known from the above-mentioned Ullmann, page 467, table 12 which is relied on and incorporated herein by reference. Precipitated silica VN3 and further precipitated silicas usable according to the invention are known from the publication “
Fällungskieselsäuren und Silikate, Herstellung, Eigenschaften und Anwendung
”, Degussa Aktiengesellschaft, September 1983.
Emulsions known from the document EP-B 0 538 555 as well as mixtures of different silane emulsions may be used as the aqueous emulsions of silanes. The entire disclosure of EP-B 0538 555 is relied on and incorporated herein by reference.
Such emulsions known from document EP-B 0 538 555 are aqueous emulsions containing organosilicon compounds, which emulsions optionally contain anionic and/or nonionic surfactants and pH-buffering substances. They contain:
(A) 1 to 80 wt. %, in particular from 1 to 60 wt. %, relative to the total quantity, of at least one alkoxysilane of the general formula
 in which
R
1
: means C
1
-C
3
alkyl
R
3
: means C
1
-C
20
alkyl, linear or branched, in particular C
8
-C
16
alkyl, phenyl
a: means 0 to 3
(B) 1 to 20 wt. %, preferably 1 to 5 wt. % of a surfactant which stabilizes the emulsion, preferably an organosilicon compound having surfactant-like properties, and
(C) contains water in a quantity of 1-95 wt. %, preferably of 1-75 wt. %, wherein the quantities by weight add up to 100%.
Apart from the compounds of the formula (I), the emulsion may also contain the partial condensation products thereof, for example dimers, trimers or other oligomers, as are known to the person skilled in the art. The pH value of the emulsion is preferably adjusted to approximately 7.5.
In a particular embodiment, a buffer substance may be added to the emulsion in a quantity of 0.1 to 5 wt. %, relative to the entire quantity of the emulsion. This substance comprises, for example, sodium hydrogen carbonate, sodium carbonate or trisodium phosphate.
In another preferred embodiment, 0.2 to 8.0 wt. %, relative to the total weight of the emulsion, of one or more known anionic surfactants are also added to the emulsion. The emulsion optionally contains 0.1 to 1.0 wt. % of a known thickener, for example from the class of cellulose or starch derivatives, likewise relative to the entire quantity of the emulsion. The emulsion may optionally contain 0.2 to 5.0 wt. % of anionic and/or nonionic surfactants, preferably organosilicon compounds having surfactant properties, as described in EP-B 0 538 555.
The emulsions are preferably produced using the silanes
(Si 208) C
8
H
17
—Si(OEt)
3
or
(Si 216) C
16
H
33
—Si(OEt)
3
.
The process according to the invention exhibits the following advantages:
The process according to the invention may be directly connected to any known process for the production of a hydrophilic silica. The drying step in the spray dryer may simultaneously be used as the step for reacting the silica with the silane. Combined spraying of the silica suspension and the silane emulsion ensures homogeneous surface modification of the silica particles and thus a narrow distribution of the degree of hydrophobization. The very short reaction time in the spray dryer minimizes the period for which the silane is exposed to elevated temperatures.
The precipitated silica according to the invention may be used for the production of defoamers and in papermaking.


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