Cleaning compositions for solid surfaces – auxiliary compositions – Cleaning compositions or processes of preparing – For cleaning a specific substrate or removing a specific...
Reexamination Certificate
2000-02-25
2001-04-24
Gupta, Yogendra (Department: 1751)
Cleaning compositions for solid surfaces, auxiliary compositions
Cleaning compositions or processes of preparing
For cleaning a specific substrate or removing a specific...
C510S444000, C510S445000, C510S446000, C510S220000, C510S224000, C510S302000, C510S309000, C510S310000, C510S311000, C510S312000, C510S313000, C510S314000, C510S367000, C510S531000, C510S532000, C510S534000, C544S163000, C544S164000, C544S159000
Reexamination Certificate
active
06221824
ABSTRACT:
BACKGROUND OF THE INVENTION
This invention relates to a process for the production of compounded acetonitrile derivatives which may be used as activators for peroxygen compounds, more particularly inorganic peroxygen compounds, for bleaching colored soils on tableware and to dishwashing detergents containing activator compounds produced by this process.
Inorganic peroxygen compounds, more particularly hydrogen peroxide, and solid peroxygen compounds which dissolve in water with release of hydrogen peroxide, such as sodium perborate and sodium carbonate perhydrate, have long been used as oxidizing agents for disinfecting and bleaching purposes. The oxidizing effect of these substances in dilute solutions depends to a large extent on the temperature. For example, with H
2
O
2
or perborate in alkaline bleaching liquors, soiled textiles are only bleached sufficiently quickly at temperatures above about 80° C. At lower temperatures, the oxidizing effect of the inorganic peroxygen compounds can be improved by the addition of so-called bleach activators, for which numerous proposals, above all from the classes of N- or O-acyl compounds, for example polyacylated alkylenediamines, more especially tetraacetyl ethylenediamine, acylated glycolurils, more especially tetraacetyl glycoluril, N-acylated hydantoins, hydrazides, triazoles, hydrotriazines, urazoles, diketopiperazines, sulfuryl amides and cyanurates, also carboxylic anhydrides, more especially phthalic anhydride, carboxylic acid esters, more especially sodium nonanoyloxy benzene-sulfonate, sodium isononanoyloxy benzenesulfonate, and acylated sugar derivatives, such as pentaacetyl glucose, have become known in the literature. By adding these substances, the bleaching effect of aqueous peroxide liquors can be increased to such an extent that substantially the same effects are obtained at temperatures of only around 60° C. as are obtained with the peroxide liquor alone at 95° C.
In the search to find energy-saving washing and bleaching processes, application temperatures well below 60° C., more particularly below 45° C. down to the temperature of cold water, have acquired increasing significance in recent years.
At these low temperatures, there is generally a discernible reduction in the effect of the hitherto known activator compounds. Accordingly, there has been no shortage of attempts to develop more effective activators for this temperature range, but so far to no real avail.
Another problem which particularly affects machine dishwashing detergents is the need to incorporate corrosion inhibitors for table silver in such detergents, particularly where the detergents contain the oxygen-based bleaching or oxidizing agents which have recently become more widespread. During the dishwashing process, silver is capable of reacting with sulfur-containing substances dissolved or dispersed in the wash liquor, because food residues, including inter alia mustard, peas, egg and other sulfur-containing compounds, such as mercaptoamino acids, are introduced into the wash liquor in the cleaning of tableware in domestic dishwashing machines. The far higher temperatures prevailing during machine dishwashing and the longer contact times with the sulfur-containing food remains also promote the tarnishing of silver by comparison with manual dishwashing. In addition, the silver surface is completely degreased by the intensive cleaning process in the dishwashing machine and, as a result, becomes more sensitive to chemical influences.
The problem of tarnishing becomes acute in particular when active oxygen compounds, for example sodium perborate or sodium percarbonate, are used alternatively to the active chlorine compounds which oxidatively “deactivate” the sulfur-containing substances in order to eliminate bleachable soils, such as for example tea stains/tea films, coffee residues, dyes from vegetables, lipstick residues and the like.
Active oxygen bleaching agents of the type in question are used above all in modern low-alkalinity machine dishwashing detergents of the new generation, generally together with bleach activators. These detergents generally consist of the following functional components: builder component (complexing agent/dispersant), alkalinity source, bleaching system (combination of bleaching agent and bleach activator), enzyme and surfactant. Under the dishwashing conditions prevailing where detergents such as these are used, not only sulfidic coatings, but also oxidic coatings are generally formed on the silver surfaces—where silver is present—through the oxidizing effect of the peroxides formed as intermediates or the active oxygen.
It is known from International patent application WO 98/23719 that compounds corresponding to general formula I:
R
1
R
2
R
3
N
+
CH
2
CN X
−
(I)
in which R
1
, R
2
and R
3
independently of one another represent an alkyl, alkenyl or aryl group containing 1 to 18 carbon atoms, in addition to which the groups R
2
and R
3
may even be part of a heterocycle including the N atom and optionally other hetero atoms, and X is a charge-equalizing anion, can be used as activators for peroxygen compounds, more especially inorganic peroxygen compounds, in aqueous dishwashing solutions. An improvement in the oxidizing and bleaching effect of peroxygen compounds, more especially inorganic peroxygen compounds, at low temperatures below 80° C. and, more particularly, in the range from about 15° C. to 55° C. is achieved in this way. The compounds corresponding to general formula (I) are normally unstable in storage and, in particular, extremely sensitive to moisture, especially in combination with other ingredients of detergents. In the course of their production, some of the compounds of general formula (I) are obtained in liquid form, for example as aqueous solutions, and can only be converted from liquid form into the pure solid with considerable losses so that their use in solid detergents, for example particulate detergents, is problematical.
Accordingly, the problem addressed by the present invention was to provide a production process by which solutions containing a compound corresponding to general formula (I) could be converted into particulate preparations so that the active substance corresponding to formula (I) could be incorporated in solid detergents without any losses. It has now been found that preparations of the type in question, which are also referred to hereinafter as compounds, can be produced by vacuum vapor drying in a mixer. In this way, drying and granulation can be carried out in the one and the same unit.
DESCRIPTION OF THE INVENTION
The present invention relates to a process for the production of a particulate preparation containing a compound corresponding to general formula (I):
R
1
R
2
R
3
N
+
CH
2
CN X
−
(I)
in which R
1
, R
2
and R
3
independently of one another represent an alkyl, alkenyl or aryl group containing 1 to 18 carbon atoms, in addition to which the groups R
2
and R
3
may even be part of a heterocycle including the N atom and optionally other hetero atoms, and X is a charge-equalizing anion, characterized by the steps of
a) introducing a suspension containing a solution of a compound corresponding to formula (I) in a solvent for that compound and a solid carrier material into a mixer,
b) drying the suspension with superheated vapor under a pressure below 900 mbar and at a drying temperature of 40° C. to below 100° C.,
c) cooling the mixture to a temperature below the drying temperature and
d) forming granules during the drying step or during the cooling of the mixture or the melt formed (if any).
The solid carrier material is preferably selected from the group consisting of alkali metal sulfates, alkali metal citrates, alkali metal phosphates, silicas, zeolites and mixtures thereof.
Compounds corresponding to formula I may be prepared by known methods, as published for example by Abraham in Progr. Phys. Org. Chem. 11 (1974), pages 1 et seq. or by Arnett in J. Am. Chem. Soc. 102 (1980), pages 5892 et seq., or by similar meth
Gonzalez Artiga
Hammelstein Stefan
Lietzmann Andreas
Nitsch Christian
Speckmann Horst-Dieter
Boyer Charles
Gupta Yogendra
Henkel Kommanditgesellschaft auf Aktien
Jaeschke Wayne C.
Murphy Glenn E. J.
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