Drug – bio-affecting and body treating compositions – Dentifrices
Reexamination Certificate
2001-12-20
2003-12-02
Rose, Shep K. (Department: 1614)
Drug, bio-affecting and body treating compositions
Dentifrices
C424S056000
Reexamination Certificate
active
06656454
ABSTRACT:
BACKGROUND OF THE INVENTION
This invention relates to the use of special surfactant granules for the production of surface-active compositions, preferably detergents, soaps and oral and dental care preparations.
1. Prior Art
Monoglyceride (ether) sulfates are acquiring increasing significance for use in surface-active compositions by virtue of their excellent detersive properties. Hitherto, they have generally been used in the form of water-containing preparations. A major disadvantage of this is that these pastes generally contain between 50 and 75% by weight of water in order to be sufficiently pumpable. On the market, however, there is a heavy demand for solid water-free supply forms which can be incorporated in particular in powder-form detergents, tooth creams or syndet soaps without having to be dried beforehand.
Solid monoglyceride (ether) sulfates obtained, for example, by drying and simultaneous granulation in a thin layer in a so-called flash dryer are known from the prior art (DE 19641275 C1). Unfortunately, the surfactants produced in this way have unsatisfactory dissolving properties in detergents.
Accordingly, the problem addressed by the present invention was to provide a solid supply form of monoglyceride (ether) sulfates which could be prepared with a little water and which would be distinguished by improved dissolving behaviour in laundry detergents, dishwashing detergents and cleaning compositions.
2. Description of the Invention
The present invention relates to surfactant granules obtainable by subjecting 20 to 60% by weight and preferably 40 to 50% by weight aqueous pastes containing monoglyceride (ether) sulfates to simultaneous drying and granulation in a fluidized bed.
The present invention also relates to the use of these surfactant granules for the production of surface-active compositions, preferably oral and dental care preparations.
It has surprisingly been found that the drying and granulation of aqueous surfactant pastes in a fluidized bed (“SKET granulation”) leads to solid supply forms of the monoglyceride (ether)sulfate which are distinguished by excellent dissolving behavior in laundry detergents, dishwashing detergents and cleaning compositions. In addition, monoglyceride (ether) sulfate granules produced in this way have an abrasive effect in oral and dental care preparations and may therefore be used as a substitute for other abrasives. This has the particular advantage that the quantity of abrasives can be reduced without any effect on abrasive performance. Bar soaps containing monoglyceride (ether) sulfate granules as surfactant component are distinguished by good foaming behavior, better stability in air and a reduced tendency towards softening.
In combination with other surfactants, especially fatty alcohol sulfates, sulfosuccinates, olefin sulfonates, alkyl and/or alkenyl oligoglycosides, a synergistic improvement in the properties mentioned is observed. In addition, where these granules are used in the described compositions, there is no need for the removal of water which would be necessary if comparable aqueous pastes were used.
Monoglyceride (Ether) Sulfates
Monoglyceride sulfates and monoglyceride ether sulfates are known anionic surfactants which may be obtained by the relevant methods of preparative organic chemistry. They are normally produced from triglycerides which, optionally after ethoxylation, are transesterified to the monoglycerides and then sulfated and neutralized. The partial glycerides can also be reacted with suitable sulfating agents, preferably gaseous sulfur trioxide or chlorosulfonic acid [cf. EP 0 561 825 B1, EP 0 561 999 B1 (Henkel)]. If desired, the neutralized products may be subjected to ultrafiltration to reduce their electrolyte content to the required level [DE 42 04 700 A1 (Henkel)]. Overviews of the chemistry of monoglyceride sulfates have been published, for example, by A. K. Biswas et al. In J. Am. Oil. Chem. Soc. 37, 171 (1960) and F. Ahmed in J. Am. Oil. Chem. Soc. 67, 8 (1990). The monoglyceride (ether) sulfates suitable for use in accordance with the invention correspond to formula (I):
in which R
1
CO is a linear or branched acyl group containing 6 to 22 carbon atoms, x, y and z together stand for 0 or for numbers of 1 to 30, preferably 2 to 10, and X is an alkali metal or alkaline earth metal. Typical examples of monoglyceride (ether)sulfates suitable for the purposes of the invention are the reaction products of lauric acid monoglyceride, coconut fatty acid monoglyceride, palmitic acid monoglyceride, stearic acid monoglyceride, oleic acid monoglyceride and tallow fatty acid monoglyceride and ethylene oxide adducts thereof with sulfur trioxide or chlorosulfonic acid in the form of their sodium salts. Monoglyceride sulfates corresponding to formula (I) in which R
1
CO is a linear acyl group containing 8 to 18 carbon atoms and preferably 12 to 14 carbon atoms, x, y and z=0 and X is sodium are preferably used.
Surfactants/surfactant Granules
In one preferred embodiment of the invention, aqueous pastes containing fatty alcohol sulfates, sulfosuccinates, olefin sulfonates, alkyl and/or alkenyl oligoglycosides as further surfactants are dried and granulated. Alternatively, the monoglyceride (ether) sulfate granules may be present in admixture with granules of fatty alcohol sulfates, sulfosuccinates, olefin sulfonates, alkyl and/or alkenyl oligoglycosides such as, for example, monoglyceride (ether) sulfate, fatty alcohol sulfate, alkyl and/or alkenyl oligoglycoside granules.
Fatty Alcohol Sulfates
Fatty alcohol sulfates are understood to be primary aliphatic alkyl sulfates corresponding to formula (II):
R
2
O—SO
3
X (II)
in which R
2
is a linear or branched, saturated or unsaturated hydrocarbon radical containing 12 to 14 carbon atoms and X is an alkali metal and/or alkaline earth metal, ammonium, alkyl ammonium, alkanolammonium or glucammonium. Fatty alcohol sulfates are known anionic surfactants which are preferably obtained by sulfation of native fatty alcohols or synthetic oxoalcohols and subsequent neutralization. Typical examples of fatty alcohol sulfates are the sodium salts of sulfation products of lauryl alcohol, isotridecyl alcohol, myristyl alcohol and the technical mixtures thereof obtained, for example, in the high-pressure hydrogenation of technical methyl esters based on fats and oils or aldehydes from Roelen's oxo synthesis and as monomer fraction in the dimerization of unsaturated fatty alcohols. Fatty alcohols containing 12 to 14 carbon atoms such as, for example, technical C
12/14
coconut alcohol sulfates and, more particularly, lauryl alcohol are preferably used.
Sulfosuccinates
Sulfosuccinates, which are also referred to as sulfosuccinic acid esters, are known anionic surfactants which may be obtained by the relevant methods of preparative organic chemistry. They correspond to formula (III):
where R
3
is an alkyl and/or alkenyl group containing 6 to 22 carbon atoms, R
4
has the same meaning as R
3
or X, n and m independently of one another stand for 0 or for numbers of 1 to 10 and X is an alkali metal or alkaline earth metal, ammonium, alkylammonium, alkanolammonium or glucammonium. They are normally produced from maleic acid, but preferably from maleic anhydride, which in a first step is esterified with optionally ethoxylated primary alcohols. The monoester-to-diester ratio can be adjusted at this stage by varying the quantity of alcohol and the temperature. The second step comprises the addition of bisulfite which is normally carried out in methanol as solvent. Fairly recent overviews of the production and use of sulfosuccinates have been published, for example, by T. Schoenberg in Cosm. Toil. 104, 105 (1989), by J. A. Milne in R. Soc. Chem. (Ind. Appl. Surf. II) 77, 77 (1990) and by W. Hreczurch et al in J. Am. Oil. Chem. Soc. 70 707 (1993). Typical examples are sulfosuccinic acid monoesters and/or diesters in the form of their sodium salts which are derived from fatty alcohols containing 8 to 18 and preferably 8 to 10 or 12
Eggers Anke
Hensen Hermann
Koester Josef
Kosboth Celia
Seipel Werner
Cognis Deutschland GmbH & Co. KG
Rose Shep K.
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