Methods of making dentifrice compositions and products thereof

Details Methods of making dentifrice compositions and products thereof Methods of making dentifrice compositions and products thereof

2000-08-18

2002-06-11

Rose, Shep K. (Department: 1614)

Drug, bio-affecting and body treating compositions

Dentifrices

C051S308000, C423S335000, C423S338000, C423S339000

Reexamination Certificate

active

06403059

ABSTRACT:

BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to methods of making dentifrice compositions and the resulting products.
2. Description of the Related Art
Conventional dentifrice compositions typically include an abrasive substance in order to remove various deposits, including pellicle film, from the surface of teeth. Pellicle film is tightly adherent and often contains brown or yellow pigments which impart an unsightly appearance to the teeth. While cleaning is important, the abrasive should not be so aggressive so as to damage the teeth. Ideally, an effective dentifrice abrasive material maximizes pellicle film removal while causing minimal abrasion and damage to the hard tooth tissues. Consequently, among other things, the performance of the dentifrice is highly sensitive to the abrasive polishing agent ingredient. Conventionally, the abrasive polishing material has been introduced in flowable dry powder form to dentifrice compositions, or via re-dispersions of flowable dry powder forms of the polishing agent prepared before or at the time of formulating the dentifrice.
A number of water insoluble, abrasive polishing agents have been used or described for dentifrice compositions. These abrasive polishing agents include natural and synthetic abrasive particulate materials. The generally known synthetic abrasive polishing agents include amorphous precipitated silicas and silica gels and precipitated calcium carbonate (PCC). Other abrasive polishing agents for dentifrices have included chalk, magnesium carbonate, dicalcium phosphate and its dihydrate forms, calcium pyrophosphate, zirconium silicate, potassium metaphosphate, magnesium orthophosphate, tricalcium phosphate, and the like.
Synthetically-produced precipitated silicas, in particular, have been used as abrasive components in dentifrice formulations due to their cleaning ability, relative safeness, and compatibility with typical dentifrice ingredients, such as humectants, thickening agents, flavoring agents, anti-caries agents, and so forth. As known, synthetic precipitated silicas generally are produced by the de-stabilization and precipitation of amorphous silica from soluble alkaline silicate by the addition of a mineral acid and/or acid gases under conditions in which primary particles initially formed tend to associate with each other to form a plurality of agglomerates (i.e., discrete clusters of primary particles), but without aggregation into a three-dimensional gel structure. The resulting precipitate is separated from the aqueous fraction of the reaction mixture by filtering, washing, and drying procedures, and then the dried product is mechanically comminuted in order to provide a suitable particle size and size distribution.
The silica drying procedures are conventionally accomplished using spray drying, nozzle drying (e.g., tower or fountain), flash drying, rotary wheel drying, oven/fluid bed drying, and the like, which often require considerable expenditures for equipment and operating costs. A similar issue is associated with other synthetically derived polishing agents, such as PCC.
Additionally, conventional abrasive polishing agents destined for dentifrice formulations have required comminution in order to reduce the particle size of the dewatered precipitated silica product down to a size that does not feel gritty in the mouth of a dentifrice user, while, on the other hand, not being so small as to lack sufficient polishing action. That is, in conventional practice, the average particle size of the silica in the reactor formed by acidulation of a metal silicate is too large for dentifrice applications and the like. To comminute dry silica particulates, grinding and milling equipment have been used, such as a hammer or a pendulum mill used in one or multiple passes, and fine grinding has been performed, for example, by fluid energy or air-jet mill. These additional dry comminution operations entail added cost and process time. Moreover, conventional dry grinding and milling equipment and methods tends to introduce impurities into the silica which can diminish the brightness, i.e., cause “graying”, of the formulation which ultimately incorporates the ground dry silica.
U.S. Pat. No. 3,506,757 to Salzmann describes liquid dentifrices comprising particulate abrasive materials, stably suspended in an aqueous liquid vehicle with the aid of a polysaccharide gum as suspending agent. Similarly, PCT published application no. WO 97/46485 describes silica having a median particle size generally around 12 to 30 &mgr;m provided in the form of a suspension, which can be stabilized using a hydrocolloid, particularly naming polysaccharides such as xanthan gum, guar gum, and water-soluble cellulose ethers. U.S. Pat. No. 5,310,543 describes liquid dentifrices containing particulate siliceous abrasive cleaning agents stably suspended in a liquid medium with the aid of a polysaccharide gum and using a liquid medium specified as being substantially free from polyol-type humectants in order to obtain satisfactory rheological properties.
Among other things, dentifrice compositions containing appropriately sized abrasive particles would be desirable that could be prepared as part of a continuous process flow and without the need for costly drying and dry milling/comminuting procedures being done on the abrasive component of the dentifrice.
SUMMARY OF THE INVENTION
The above and other objectives, advantages and benefits are achieved by the present invention which is directed to dentifrice compositions made with an abrasive composition ingredient comprised of water-insoluble abrasive polishing agents suspended in a liquid medium based on humectant. The resulting dentifrice compositions have unique attributes, such as enhanced TAPPI brightness imparted to the abrasive component as processed for incorporation into the dentifrice.
In one embodiment, the invention concerns a method for making dentifrice compositions by a continuous, integrated process without need for performing dewatering procedures on the ingredients of the dentifrice before dentifrice formulating. In particular, the abrasive component used as a raw material in making the dentifrice according to this invention is conveniently and cost-effectively provided as a stable, pumpable slurry of silica, never dried, by dispersing filtered silica cake obtained directly from the precipitation reactor in a humectant. In particular, capital and energy costs are saved by eliminating drying-dewatering operations in the processing of the silica abrasive component used in making a dentifrice composition according to this invention. Further, the comminution requirements for the abrasive particle content of the inventive dentifrices are reduced, if not completely eliminated in some cases, by the effective performance of comminution concurrent with synthesis of the abrasive material to be used in the dentifrice in a common reactor system in the practice of this invention. The water-insoluble abrasive particulate product of the reaction is provided with the requisite particle size suited for oral cleaning compositions to eliminate the need for drying and comminuting dry silica solids after filtration. While not desiring to be bound to any particular theory at this time, it is postulated that the Theological properties of the abrasive compositions used in making dentifrices according to this invention are superior, at least in part, due the avoidance of agglomeration of particles otherwise incurred by the silica particles during conventional silica particle drying procedures. By contrast, the dentifrice compositions made according to this invention contain silica particles that retain or essentially retain the original structure and chemistry of the reactor silica and avoid changes in surface hydroxyl group type and density. In this regard, the undried abrasive particles used in dentifrices made according to this invention show improved TAPPI brightness values as compared to abrasive particles derived from processing involving abrasive particle drying a

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