KR880001982B1 - Dentifrices containing functional agglomerated speckles - Google Patents

Abstract

Functional agglomerated speckles for incorporation in dentifrices include agglomerates of a water-insol. powd. functional material, usually polishing agents, and water-insol., EtOH-sol. Et-cellulose. Agglomerates were prepd. from 5 pts. Et cellulose and 95 pts. calcined alumina. The agglomerates were screened to give angular shaped speckles with the ratio of max. length to max. width of 1:1-2 and particle sizes of 30 to 60 (U.S. sieve series). Five pts. of speckles were blended with 95 pts. dentifrice base (transparent or translucent).

Description

Toothpaste with functional aggregation spots

FIG. 1 is a perspective view of the gelled toothpaste tube of the present invention comprising a peeled cap and toothbrush, FIG. 2 is an explanatory view of the device of the present invention for producing a spotted toothpaste from a toothpaste composition and speckles, and FIG. Is an enlarged perspective view of the site of the "Speckling apparatus" of the present invention, which is applied to the gel-like flow or ribbon, and FIG. 4 is an explanatory view of another apparatus of the present invention for producing a spotted toothpaste, and FIG. Is a magnified perspective view of the "spot apparatus" of FIG. 4 applying gel flow or ribbon to the gel.

The present invention relates to functional flocculation spots for toothpaste mixing.

In particular, the present invention relates to spots prepared from water-insoluble, dense functional substances such as dental polishes and water-insoluble ethanol-soluble ethylcellulose, preferably with water-soluble binders such as polyvinyl pyrrolidone and toothpastes containing these spots. It is about.

The present invention also relates to such spots and methods and devices for making such toothpastes and to such toothpastes packaged in dispensing containers such as transparent or translucent containers in which spots in transparent or translucent gelled toothpastes can be observed from the outside. . To achieve the required visual effect, the spots will typically have to be in opposition to the rest of the toothpaste.

Prior art cream toothpastes and gel toothpastes with contrasting color spots are known. In some cases such spots exist primarily for aesthetic effects, but these spots may be based on functional ingredients such as polishes. In the past, various flaky toothpastes were distinct at first, but contained spots that became fine during brushing.

While such products are consistent with the technical level, they have also been found to be easily spotted and distinguished, but later found to be required for the production of other forms of ignited toothpastes, such as the toothpaste of the present invention, which are fine during brushing as well as initially. Toothpastes containing visible and distinctly completely insoluble varnish factor are known in the prior art.

The use of binders in the preparation of dental spots is described, and methylcellulose and polyvinyl pyrrolidone (PVP) are described as water-soluble binders. Methylcellulose, however, is water soluble and therefore does not provide spots that remain intact during prolonged processing. Toothpastes containing encapsulated sweeteners are known in the prior art and ethyl cellulose is described among various other materials used to coat sweeteners to make spheres.

Water soluble and water insoluble binders used in dental spots are described together in this prior art, but ethyl cellulose is not mentioned here.

Paste toothpaste formulations in which the visible cohesion factor of dental polish is dispersed therein are known, and the advantages of water-soluble and water-insoluble coagulants or binders are recognized, but ethyl cellulose has been suggested as a binder in such literature. none.

Fine encapsulation of sodium fluoride with lower alkyl cellulose such as ethyl cellulose and dispersion of this capsule in toothpaste have been proposed, but this suggestion has nothing to do with flocculating material for preparing dental spots.

The present invention utilizes water-insoluble but ethanol-soluble ethylcellulose as a flocculant of functional water-insoluble powdery substances prepared with toothpaste spots of improved properties.

The preceding spots made with water-soluble binders such as methylcellulose are prepared from the formulations above if the sparkling toothpaste, which can occur in the case of a mechanical failure of the manufacturing equipment, stays in the manufacturing equipment for too long. It may disintegrate during processing after mixing with other toothpaste components, such as in a gel or pasty medium. This loss of spots can occur because these toothpastes contain water, which can dissolve the spot's water-soluble binder and cause separation of the spot component particles.

Dissolution of the binder can be minimized in this case by an immediate process, but can result in product loss if improper detention of the filling line causes an increase in processing time.

As described in the prior art (prior art does not describe ethyl cellulose), toothpaste spots, usually made of water-insoluble binders, are clearly identified when dispersed in gelled or paste toothpastes, which is often desirable. This may be the case, but not for toothpaste intended for use by people with sensitive gums.

Ethyl cellulose, which is used as a binder for functional spots according to the present invention, maintains spots in a water-soluble toothpaste medium satisfactorily even after processing for a long time after blending the spots in the toothpaste. However, due to the presence of toothpaste components which tend to soften spots during storage, such as flavoring agents and, in some cases, surface active agents, the spots in toothpaste soften significantly during storage, making these spots complete and independent until the product is used. Although they maintain a distinctive appearance, these spots become fine and easily disintegrate during brushing.

PVP in some preferred formulations, such as toothpastes that may contain smaller amounts of flavorants (and dental cleaners and other solvents or lipophilic substances) or toothpastes containing substances that have low solubility properties (for ethyl cellulose). The presence of a water-soluble cobinder such as this makes it possible to obtain the required micronization ability. Again, due to the presence of ethyl cellulose, spot integrity is maintained.

Powdered water-insoluble functional substances (or mixtures of such functional powders and water-soluble binders) are "wet" with a water-insoluble ethyl cellulose solution in a volatile solvent, compressed, and then converted into granular form and dried. The preparation, preferably by means of the preparation, can be adjusted to add to the toothpaste stream, allowing the spot to be uniformly dispersed and adhered to the toothpaste, and preferably using a particular device.

In the present invention, the functional flocculation spots for toothpaste formulations consist of a water insoluble powder functional material and a water insoluble ethanol soluble ethylcellulose, optionally agglomerates in which a water soluble binder is also present.

The functional coagulation spot consists of two main components, a water insoluble powder functional substance and a water insoluble, ethanol-soluble ethyl cellulose. The former material can be specifically deleted as a functional bodying agent and the latter material as a binder. Colorants such as pigments, fungicides, ion exchangers, polymers (which may contain other active ingredients, sometimes water-soluble substances), preferably various functional substances which are water insoluble or at least slowly soluble may be used. However, the functional base material for spots is a varnish, and a functional material composed mostly of it is very preferable. Preferred examples of brighteners commonly used in the form of dry powders for producing flocculation spots are dicalcium phosphate, tricalcium phosphate, insoluble sodium metaphosphate, alumina, silica, magnesium carbonate, calcium carbonate, calcium pyrophosphate, bentonite and zirconium silicate and Suitable mixtures thereof.

Although both anhydrous or calcined forms such as lit alumina and hydrated forms such as dicalcium phosphate dihydrate can be used, anhydrous or calcined materials are more preferably used.

Usually the nodule is preferably opaque, so the refractive index (including other components as well) does not need to match the refractive index of the toothpaste herbicide, but a "transparent" polish having a matching refractive index such as 1.44 to 1.47 is used as a polishing agent. Of course, it is used to prepare a clear gel toothpaste body containing, but may also be used to prepare transparent or translucent spots. Such "transparent" varnishes include colloidal silica and include materials sold under the Syloid trademarks such as Syloids 63, 65, 72 and 74, and Santocel trademarks such as Santocel 100 and Zeo's 49, 113 and 119 and Zeodent. . Synthetic alkali metal aluminosilicate complexes may also be particularly useful because these compounds have refractive indices that approximate the refractive index of dental bases, including water, glycerol, sorbitol and gelling agents commonly used in toothpaste preparation. to be.

The water-insoluble powdered functional material used to prepare the spots of the present invention is usually in the initial particle size range of 0.5 to 20 microns, preferably 1 to 10 microns, more preferably in the range of 2 to 8 microns. However, larger particle sizes may be used in some cases where the flocculation process tends to reduce the particle size of some powders, as may occur during mixing before actual flocculation begins.

The spot binder for the present invention is ethyl cellulose. This effective binder is water insoluble but soluble in ethanol and gradually dissolved in water-soluble glycerol-sorbitol media such as flavoring agents and surfactants commonly present in the toothpaste of the present invention and materials contained as solvents thereof. Such ethyl cellulose usually has an ethoxy content range of about 45-50%, with 48-50% or 48-49.5% being preferred.

Preferred ethyl cellulose, such as that sold by Dow Chemical Campanile under the trade name Ethocel Standard 10 Premium Ethyl Cellulose, has an ethoxy content in the range of 48.0-49.5%, a viscosity of 9-11 centipoise, and a water content of 2%. Hereinafter, chlorine is 0.15% or less as NaCl, and ash content is 0.15% or less.

Ethyl cellulose resins suitable for use as spot binders of the present invention are commercially available as white to light tannin color granule powders in which an etherification reaction is carried out so that 2.25 to 2.58 ethoxy groups per anhydroglucose unit are present, which is 45.0 to 49.5% by weight. It will have a oxy content. Of these two kinds of ethyl cellulose, the preferred material for the practice of the present invention has an ethoxy content in the range of 48.0 to 49.5%, and a less preferred material is an ethoxy content in the range of 45.0 to 46.5%. Such products are, of course, obtained in different viscosity ranges, the former being usually at 3 to 110 centipoise and the less desirable materials at higher viscosities.

Preferred or "standard" grade ethylcellulose tends to be soluble in aromatic hydrocarbons, hydroaromatic hydrocarbons, chlorinated aliphatic hydrocarbons and seawater. It also contains aliphatic monohydric alcohols such as ethanol: cycle monohydric alcohols such as benzyl alcohol, phenyl ethyl alcohol and pine oil: ether alcohols such as glycol ethers, ethers such as diethyl cellosolve: especially isopropyl acetate and secondary amyl acetate Esters such as acetates such as and hydroxy acid esters such as methyl salicylate; And soluble in ketones such as cyclohexanone and acetophenone.

In general, less preferred or "medium" epoxy grade ethyl cellulose is less soluble than standard grade, and thus may be more suitably used when there is a greater amount of soluble material on the toothpaste structure.

Although there are many water-soluble binders used to prepare mixed binders which are sometimes preferably used for the production of spots of the present invention, gum acacia; Gelatin; Natural and modified starch; Alkali metal carboxymethyl cellulose; In particular sodium carboxymethyl cellulose; Polyethylene glycol; Sugars such as glucose and sucrose; Methyl cellulose; Carboxyethyl hydroxyethyl cellulose; Alginates, in particular sodium alginate; Polyvinyl alcohol; Hornheads, preferably Irish moss; Xanthan gum; Gum tragacanth; And PVP.

PVP is stable in the presence of ethyl cellulose, mixed with ethyl cellulose to prevent excessive spillage from the spots formulated as a binder, and mixed so that the total amount required for various toothpaste preparations can be used. It is used to adjust the compounding properties of the compounding agent to adjust the ethyl cellulose / PVP ratio.

It is also important to note that the blending agent properties in these spots should not be soft enough during storage of the blended toothpaste to the extent that they are very hard or hard enough that the spots do not sufficiently dissolve during the process, or that the spots become fine before the toothpaste is used. will be. If they are not softened sufficiently, they cause streaks in the tube or during release, but if necessary, control streaks may be obtained in some cases by increasing the PVP to adjust the ethylcellulose / PVP ratio.

PVP is usually in the molecular weight range of 30,000 to 50,000, and preferably used in the present invention is PVP having a molecular weight of about 40,000.

Such products, commercially available from GAF Corp. under the trademark Plasdone, such as Plasdone K 29-32 and K26-28, are assigned an average molecular weight by the indicated K value, with K-30 corresponding to about 40,000 molecular weight.

PVP is obtained as a pale powder containing less than 5% moisture, 12.6 ± 0.4% nitrogen, less than 2 ppm arsenic and less than 20 ppm heavy metals. It is soluble in cold water and soluble in various organic alcohols, acids, ether-alcohols, ketone-alcohols, chlorinated hydrocarbons, esters and ketones, but insoluble in hydrocarbons, some ethers, chlorinated hydrocarbons, ketones and esters.

This material can be used in combination with many synthetic and oil-based cleaning agents, including those commonly used as dental cleaning agents, including various natural and synthetic resins, inorganic salts and sodium higher fatty alcohol sulfates and poly-lower alkoxylated alcohol sulfates.

While the best spots can be expected to be made from the most insoluble binder material, ethyl cellulose, as described herein, maintains individuality and completeness during manufacturing and storage, but also during toothbrushing use. It has been found that they produce spots of ideal properties that are fully refined.

If necessary, the speckle properties may be altered by changing the ethoxy content of ethylcellulose and / or by combining it with other fully water-insoluble binders of known form.

Similarly, if there is no lipophilic content in the toothpaste and the spots are difficult to micronize during storage, a water-soluble binder such as PVP may be used with ethyl cellulose to increase the ductility of the spots. Such spot control can also be implemented by using more water-soluble binders or more such binders, or by modifying these molecular weights (such as reducing the molecular weight of PVP).

Spot properties can also be controlled by adjusting the ratio of functional material to binder as will be discussed below. Thus, the nodules are stable during mixing and during processes such as degassing and filling, but are quickly destroyed after toothpaste cream has been extruded from the container or, if necessary, prevented such fractures, making it harder for the user to squeeze it. It can also be manufactured to feel somewhat solid from the nodule. Generally, the spots will be fully refined at the time of use, but it is highly desirable to retain the uniqueness of these spots in the toothpaste.

The binder usually has the same particle size as the functional powder material of the speck, especially when the powder material is partially squeezed to form nodules.

Since the spots are usually prepared using an alcohol solution of ethylcellulose, their particle size may be relatively insignificant. However, if a water soluble binder is present, it is believed that the size is preferably equal to the size of the functional material.

Sometimes spots with white or colorless and translucent or transparent or such appearances may also contain a suitable amount of dye or pigment or a mixture of dyes and / or pigments to give a color. Strong colors, non-toxic dyes or pigments of suitable color, usually Munsell chroma 4 or more and Munsell values in the range of 4-7 may be used, and in some cases weak or pastel pastels may be satisfactory or desirable. have.

It is usually best to use dyes or pigments applied for drugs and cosmetics (D & C) or for food, drugs and cosmetics (FD & C).

Representatives of suitable dyes include D & C Red Nos. 2, 3, 6, 7, 8, 9, 10, 11, 12, 13, 19, 30, 31, 36 and 37; D & C Blue No. 1; FD & C Blue numbers 1 and 2; FD & C Red Numbers 1, 2 and 3; FD & C Yellow No. 5: Cosmetic green oxide; And cosmetic red oxides.

Pigments of the aforementioned dyes known as lakes are also suitable for use for spot coloring, but usually dyes are more preferred.

The pigments mentioned often consist of a dye supported on a fine powder insoluble carrier, and in the medium being colored this pigment is dispersed rather than dissolved. The particle size of the pigment used may be in the range described above for the brightener or may be the same particle size as the binder. The particle size may be finer, such as in the range of 0.01 to 1 micron.

Dye particle sizes may be similar, but since the dye is usually used dissolved in water or in a solvent and is preferably oil soluble and soluble in a suitable solvent, the powder or particles may be easily dissolved in the solvent in which the dye is selected. Particle size is not that important as long as it is small enough.

Spots of the present invention may be prepared by any suitable method, either wet or dry. When ethyl cellulose is the only binder and wet formulation is used, it is preferred to first combine ethyl cellulose in dry powder form first as a brightening agent and, if necessary, as a dye or pigment and ethanol. Water and / or a lipophilic solvent may be present with ethanol, and dyes or pigments for coloring the spots may also be added. Alternatively, often ethanol solutions of ethylcellulose preferably contain suitable dyes or pigments, and the brightening agent may be mixed therewith.

The composition ratio is maintained so that the required spots of the composition can be obtained, and the solvent ratio is usually 5 to 50%, preferably 5 to 25% of the mixture. The dispersion may be prepared using a Hobart mixer, a Dravo pan, or other suitable mixing device or granulator for wet powder, and the order of addition of various components of the dispersion may be adjusted to the most suitable state of the mixing device or blending device used. It may be. Preferred methods of making the spots include a "wettable" mixture of a brightener and ethyl cellulose (including dyes or pigments, if used), typically in the range of about 150 to 2,000 microns (about 10 to 100 times in the United States Sea-Bube sequence). It is pushed into a screen with uniform openings in the sheave range and the “extruded” nodules are then dried normally in air or in a drying furnace.

Instead of the screen, other devices such as extruders may be used to prepare pellets by extrusion or other mixtures and then the resulting particles may be dried. Its particles are classified into particle size ranges ranging from 10 to 80, preferably from 40 to 80 and more preferably from 30 to 60 (US-Si-Bu family). Of course, if the wet material is produced in a Dravo pan, screen extrusion or other extrusion may be omitted.

In general, when the particle size is greater than 2,000 microns (10 sheaves), the substance is inadequate to put into the user's mouth, and when it is about 177 microns in diameter (80 sheaves) or less, it cannot be easily identified. It cannot be an interesting appearance.

Instead of the wet granulation method, it can also be used as a dry or slug method, where the spot components squeeze into large tablet sizes, destroy such tablets, and separate particles in the required particle size range from other particle size materials.

In such tablet preparation methods, it may also be desirable to use water-insoluble lubricants such as talc, magnesium stearate, calcium stearate or stearic acid, which may promote aggregation.

Similarly, such materials and other water insoluble auxiliaries may also be added when wet granulation methods are used. Although it is preferable that the prepared spots are dried without moisture, the moisture content of up to 10%, such as 1 to 5%, does not have any serious adverse effect on the spot properties.

The proportion of water-insoluble powdered functional substances, such as dental polishes, and binders, such as ethylcellulose or cellulose and water-soluble binders, in the spots, is characterized by the fact that the binder is a minor component of the spot, and the powdered substance is the main component (such as paints and It should also be formed to achieve the presence of other substances).

Generally, dental polishes or functional substances are 75 or 80 to 98%, preferably 85 to 97% of the spots on dry basis in the absence of water and ethanol or other solvents, and the binder or binder formulation is 2 to 20% of the spots. Preferably 3 to 15% and the colorant is 0 to 5%, such as about 0.05 to 1% of the spot.

When a binder blend is used, the ratio of ethyl cellulose / water soluble binder (PVP) is from 1: 10 to 10: 1, preferably from 1: 5 to 5: 1, more preferably from 1: 2 to 2: 1 And most preferably 1: 2 to 1: 1, such as 2: 3.

In the present invention, the toothpaste can be any product of the toothpaste dispersed in the relation to maintain the independence, individuality and discernment of the spot mainly acting as a spot medium while showing the normal toothpaste function.

Opaque dentifrices are useful as the spotting medium of the present invention, but it is highly desirable that the dentifrice is in a form that is transparent or translucent and usually specified as a gelled material.

Toothpastes usually consist of flavors and / or colorants, along with water, moisturizers, gelling agents, dental cleaning agents and varnishes. Various functional additives include fluorides, stabilizers, tooth decay agents and antibacterial compounds.

Preferred water for use is deionized water, but tap water including hard water and soft water may also be used. Gelling agents are usually water-soluble natural or synthetic rubbers or rubbery materials, examples of which include horn starch, gum tragacanth, xanthan gum, alginate, alkali metal carboxymethyl cellulose (preferably sodium carboxymethyl cellulose), Hydrophilic colloidal carboxyvinyl polymers such as those sold under hydroxymethyl carboxyethyl cellulose, polyvinyl pyrrolidone, starch and under the trade names Cabopol 934 and 940.

Although various polyols can be used as humectants, preferred polyols are compounds having 3 to 6 carbon atoms and 3 to 6 hydroxy groups per molecule, examples of which include glycerol and sorbitol. Glycerol is usually about 99% or more pure in liquid form, and sorbitol is generally used as a solid, often in 70% aqueous solution (70% sorbitol, 30% water). The three mentioned ingredients may be considered the main ingredients of the toothpaste base, but flavors and detergents may also be combined.

Such detergents may include soap, but generally synthetic organic surfactants are used that are not soaps having cleaning properties. Anionic types are used as such detergents, but nonionic detergents are also useful, amphoteric detergents may be used, and in some cases cationic detergents may be used.

Particularly useful are anionic detergents, which have good cleaning and bubble-forming properties.

Typically, such compounds will contain hydrophilic and lipophilic moieties, and the lipophilic moiety usually has 10 to 18 carbon atoms, preferably 12 to 16 carbon atoms, and the hydrophilic group is usually sodium, potassium or the like. Alkali metal or ammonium or lower alkanol ammonium. Examples of such suitable anionic detergents include higher fatty acid monoglyceride sulfates such as sodium salts of monosulfated monoglycerides of hydrogenated coconut oil fatty acids; Higher alkyl sulfates such as sodium lauryl sulfate; Water-soluble salts of alkylaryl sulfonates such as sodium linear dodecyl benzene sulfate (generally alkali metals, preferably sodium or potassium); Higher alkyl sulfoacetates; Higher fatty acid ester 1,2-dihydroxypropanesulfonate; Fully saturated higher fattyacylamides of sodium salts of sulfated polyethoxylated alcohols and lower aliphatic amino carboxylic acid compounds such as N-lauroyl sarcosine, and all sarcosine compounds are preferably free of soap or similar higher fatty acid substances. Sodium, potassium and ethanolamine salts of N-lauroyl-, N-myristori- and N-palmitoyl sarcosine which are absent.

Among the nonionic detergents, ethoxylated sorbitan monostearate having about 20 moles of ethylene oxide per mole; Pluronics of ethylene oxide with propylene oxide and propylene glycol; Polyethoxylated higher fatty alcohols such as Neodols (23-6.5 and 45-11); And α-olefin oxides containing 10 to 20 carbon atoms, heterogeneous mixtures of polyhydric alcohols having 2 to 6 carbon atoms with 2 to 6 hydroxy groups and ethylene oxide or ethylene oxide and propylene oxide Olefin oxide condensation products are useful. Quaternized imidazoyl derivatives such as Miranol C ₂ M and other miranols represent useful positive detergents, and quaternary ammonium halides such as dimethyl disetyl ammonium bromide represent cationic detergents.

Various brighteners dispersed in toothpaste bases (or detergents and other auxiliaries in addition to the bases) have been mentioned above for spot shape conversion.

Also useful as a substance in this group are finely divided synthetic silicas such as those sold under the trade names Cab-O-Sil M-5, Syloid 244, Syloid 266, Aerosil D-200, zeosyl 200 and Zeothix 265. It is used as a small amount of polish agent to less than 9% by weight, and the base agent is precipitated and gelled to increase the transparency of the toothpaste.

Toothpastes of the present invention usually contain suitable flavoring and / or sweetening agents, and examples of flavoring agents include flavoring oils such as spearmint, peppermint, winter green, sasafras, crova, sage, eucalyptus, cinnamon, lemon and orange And examples of sweetening agents include sucrose, lactose, and saccharin.

Preferred for fluorine charging also include sodium fluoride, stannous fluoride, potassium fluoride, potassium stannous fluoride, sodium hexafluoro stannate, stannous chloro fluoride and / or sodium monofluorophosphate. Can be mentioned.

As a flavoring substance, various well-known essential oils, mainly terpene; Ester; It contains alcohols, aldehydes, ketones and aromatics, many of which have aromatic odors and aromas.

Flavor is a continuous physical and physiological response obtained by the presence of a substance in the mouth, which often has a primary importance, but odor and sensation, and aromatics are not surprising. .

In this case, as mentioned earlier in the Solubility Review of Ethyl Cellulose, such a substance may slowly dissolve ethyl cellulose in the presence spots by the dissolved substance in the flavoring material, causing softening of the spots but not causing them to collapse. Not characterized by chemical properties and facts.

For example, terpenes, which are hydrocarbons and constitute the main class of perfumes or flavorings, are found in many other flavors as mentioned above (as flavor oils) and in other materials known in the perfume and flavoring arts. As it will serve as an excellent solvent for the present invention ethyl cellulose.

The flavor essential ingredient in the toothpaste composition is used to soften the ethylcellulose spots and to refine them, thereby achieving the object of the present invention without the need to add other ingredients to the toothpaste or spots for this purpose. In addition, because relatively small amounts of flavorings typically present in toothpaste, and thus the lipophilic portion of the flavor is often lowered, due to the relatively low mass transfer rate for the "solvent" material, especially because of the gelling properties of the toothpaste, the feed rate is reduced. The softening of the required spot particles usually proceeds slowly. Thus, even when the toothpaste is starting to soften double ethyl cellulose, the flavourant of the ethyl cellulose becomes saturated immediately so that it no longer dissolves ethyl cellulose rapidly. do.

After the usual time that the toothpaste is consumed in storage prior to sale and use, often about two weeks and more (which is required for certain toothpaste components to mature and improve flavor and product homogeneity). As a result, the spots are miniaturized but remain discernible.

While earlier mentioned ethyl cellulose binders, sometimes water soluble binders such as PVP will also coexist, and mention should also be made of such spots and spotted toothpastes. In these products, ethyl cellulose forms spots until ethyl cellulose is dissolved by lipophilic substances in the toothpaste, and PVP reduces the amount of ethyl cellulose used, and lower amounts of soluble flavors and other It will help to soften the spots in toothpaste containing lipophilic substances as needed.

Flavors, especially aromatics, which have a complete solvent effect on ethylcellulose, are considered to be the most important gentle solubilizing ingredients for this toothpaste, but surface-active ingredients containing an aromatic moiety may also exhibit significant dissolution effects. In addition, its wetting activity may enhance the migration of contents in the toothpaste tube, thereby increasing the dissolution rate of ethyl cellulose.

In addition, the formulation of other ingredients of toothpaste, including some sweeteners and basic ingredients, can further increase the dissolution of ethylcellulose as needed without increasing the pre-softening of the spots.

Colorants as described above with regard to the spots usually have to be used in smaller amounts in order to prepare a base contrasting to the spot.

Toothpaste may be added with a variety of other auxiliaries, including preservatives, silicones, chlorophyll compounds and ammonialation materials. In the case of preparing a transparent or semi-transparent gelled toothpaste, the chosen gloss should be a gloss having a refractive index that closely matches the refractive index of the residual toothpaste medium.

Of course, in such a transparent gel-like preparation, the residual amount of insoluble matter that clouds the gelled material is usually minimized. When adjusting the pH of the toothpaste, it is preferable that the pH is in the range of 3 to 10, more preferably 3.5 to 5 in the presence of stannous ions, and organic acids such as ions, citric acid, malonic acid and fumaric acid. 4.5 to 7 may be used if present.

In the toothpaste of the present invention, the dental polishing agent is uniformly dispersed together with the dental cleaning agent already added in duplicate in the basic agent of water, humectant, and gelling agent and the required amount of flavoring agent. Subsequently, also preferably, the spot containing the brightener (this polish is usually in a different form from the polish in the toothpaste body) is usually 0.1 to 10%, preferably 0.5 to 5%, more preferably 1 to 3% of the toothpaste. And most preferably, it is uniformly dispersed in the toothpaste in an amount of 1.5 to 2.5%.

Toothpaste bases are usually about 5-30%, preferably 10-25%, and preferably 10-20% of water; About 20 to 70%, more preferably 45 to 65%, and most preferably 50 to 60% of a moisturizer, preferably a polyol moisturizer and about 0.1 to 5%, preferably 0.1 to 1%, and more Preferably from 0.2 to 0.5% of a gelling agent. A moisturizer is preferably a mixture of glycerol and sorbitol, with a glycerol content of 5-40%, preferably 20-30%, and sorbitol content of 5-50%, preferably 25-35%, of the toothpaste base. Preferred gelling agent is sodium carboxy methyl cellulose, and the preferred amount of use is about 0.3 to 0.4%.

The toothpaste content is usually from 0.5 to 5%, preferably from 0.5 to 3%, with sodium lauryl sulfate being preferred as such a detergent. The polishing agent in the toothpaste base is usually 10 to 40%, preferably 15 to 30% and most preferably 20 to 25%, excluding the polishing agent in spots, which contains Syloid 244 silica which is also used for sedimentation. Include. Various other materials, including flavorings (usually 0.5-2%), colorants, preservatives, sweeteners and dental hardeners (fluorides), typically do not add up to 10% toothpaste, preferably 2-7%.

The use of various components in the proportions within the ranges given for the spots and the medium in which they are dispersed gave a product of interest that is stable during storage and that the spots are uniformly and interestingly dispersed.

Although it is relatively simple to prepare a flammable toothpaste after first preparing the spot, it is important to note that the mechanical stirring at the lowest speed should be performed to prevent or delay the collapse, softening and dissolution of the spot in the toothpaste.

Although lipophilic substances and residual solvents, such as those in flavor oils, slowly dissolve ethyl cellulose, it is not considered that the dissolution is increased by vigorous stirring in the process.

If the toothpaste is elevated during this mixing process, it is more important to reduce the agitation due to process manufacturing limitations. However, when ethyl cellulose binders or combination binders are used in the preparation of spots, manufacturing restrictions may be relaxed, but care must be taken continuously. Suitable devices for dispersing the spots in the toothpaste may be conventional Banbury mixers or Dough mixers running at low speeds, but may be operated gently if they can be adjusted to prevent complete destruction, dissolution or collapse of the spots. It can also mix using a blender. When such a mixer is used, the mixing braiding speed should normally be about 1 to 5 r.p.m, and the mixing will be finished in 1 to 5 minutes. After compounding is finished; The toothpaste is degassed and filled in a container such as a transparent elastic or inelastic tube. If a vacuum is applied during the mixing process, the degassing process may be omitted.

Although the manufacturing apparatus and method are standard preparations for the ignition dentifrice, it is much more preferable to use the recent invention method which promotes the mixing of the gelled toothpaste body without facing the excess agitation.

Such preparations and apparatus and other features of the invention have been described in the remainder of this specification, and the invention can be readily understood from the following description taken in conjunction with the following drawings.

1 shows a transparent walled container 11 made of a transparent polymeric material (PVC), including a toothpaste body 13, a shoulder 15, a thread neck-17 and a lid 19 separated from the tube.

It is desirable to prepare a packaged toothpaste using a deformable tube of transparent or translucent synthetic organic polymeric material, such as polyvinyl chloride, polyethylene, polyvinylidene chloride or similarly ignitable toothpastes of external appearance. Although not required, inelastic opaque tubes such as aluminum or other metal tubes may also be used.

As described, some toothpaste 21 is supplied from the tube 11 through the neck 17 onto the brush of the toothbrush 12. Toothpaste clearly shows inventive spot 23 in a continuous toothpaste medium 25. It should be noted that these spots are easily visible but are refined from scratch. During tooth brushing these spots break into small materials of roughly the same particle size as the polish component. Of course, the spot gloss also has a function of cleansing it together with the gloss in the gel toothpaste.

In Figure 2, various components of the toothpaste composition, including bases, gelling agents, brightening agents, flavoring agents, coloring agents, cleaning agents, preservatives and other auxiliaries, are optionally mixed together under vacuum to produce a composition, A gelled material preparation container 111, in which a Hobart or Dopp mixer is preferably used, is shown, in which a flammable toothpaste is added to the prepared composition by adding a spot such as a spot based on a toothpaste polish, preferably a functional method. To manufacture. The variable speed motor and / or drive 113 operates the positive displacement pump 115 at an adjustable speed to move the gelled material to the outlet 117 and to extrude or discharge the gelled material into the planar ribbon or other suitable fluid 119 through a rather limited planar orifice. Here, the spot 121 is attached to a certain piece or granule form.

Pump 115 may be fixed to adjust the gel material charge rate, or by adjusting the charge rate of the spots, thereby continuously adding the necessary proportions of spots on the flowing gel material.

It is preferable to use pump 115 with little or no shearing action so that the gelled material can maintain homogeneity (viscosity), and a screw pump having an elastic wall such as a Moyno type pump is preferable.

The gel-load outlet or extruder 117 is preferably present in a walled vessel or vessel 123 and is typically positioned so that a ribbon of gel material containing spots on its surface made in such a vessel is located near the center of the vessel. Vertically away from the bottom, it may be discharged through the central outlet 125.

The spots added to the gelled toothpaste at the above-mentioned ratios are contained in the absorber 127, which includes a speed regulator 131 and preferably with a helix-type adjustable flow rate feeder 129, which feeds the spots through the outlet 133. Emitted to the funnel-type direction control device 135 at a controlled rate, where it forms the required discharge flow of spots, forming a descent flow or guten when these spots leave, coinciding with the gel material ribbon exiting from outlet 117 Preferably, the spots are dropped completely vertically so as to deposit on or adhere to the gel material ribbon so that the spots are all in contact with the gel material.

Preferably the spot curtain covers almost the entirety of the gel material ribbon width, for example 40 to 95%, preferably 60 to 90%, the curtain being too wide and the result that any part of the spot deviates from the ribbon. Should not cause. However, when the cuppen width is possible, it is preferable to be slightly narrower than the reebok width such as 80 to 90%.

Lines 137, 139, and 141 are connected to vacuum sources 143 and 145, respectively, and require the use of a vacuum to prevent air bubbles from entering the toothpaste, but if the process is carefully processed, vacuum is used. It is also possible to prevent the mixing of such bubbles without doing so.

After the spot blast has passed through outlet 125, a pump 147, preferably a screw pump, such as a Moyno pump, is operated by a variable speed motor 149 and the product is gently pumped into Kenics' fixed-bed mixer 151, Here, the mixture is gently mixed and uniformly mixed without disintegrating or dissolving spots.

The blend is then conveyed via line 153 to receiver 155, which may be a feed tank for the tube filler not described in this figure.

In FIG. 3, the gel material supply device 157 contains the planar opening 161 together with the transfer pipe 159 and the nozzle portion 117. The opening of the gel material charging device and its exposed exposed area may be adjusted. Therefore, the supply direction can be changed as necessary and the discharge angle can be changed, but the supply direction must have a horizontal component, and 0 to 45 degrees are usually used, such as 10 to 30 degrees from the horizontal.

The square orifice can also be changed in size to further limit, but care must be taken to maintain the gel material ribbon cohesion so that the ribbon does not become thin enough to escape gel strength. Usually it can be used 1mm to 1cm, such as 2 to 6mm.

The gel material flow or ribbon should be oriented so that the spot flow or curtain will drop exactly on it, preferably the spots fall almost vertically and the gel material will move in the horizontal component direction, causing the gel material to drop. It is a case where it passes underneath and comes into contact with and sticks to it. Gel material base 163 is shown to fall to the right in the downward direction while spot 165 falls onto ribbon 163 from outlet 167 of directional device 135 (FIG. 2).

4, there is shown a container 211 for preparing a gel material similar to that of FIG. 2 and having a similar function. Valves 213 and 215 in line 217, together with the adjustable speed change pump 219, will recycle the gelled material to the mixer if necessary. Lines 220 and 221 and Valves 222 and 223 are used to release gel toothpaste (or paste toothpaste) for the preparation or cleaning of spotless toothpaste.

When the valves 215, 222 and 223 are closed and the valve 213 is opened and the gel pump 219 is opened and the lines 225 and the valve 227 are opened, the mixing apparatus 211 containing the gel toothpaste and these apparatuses control the gel material. At a rate through the gel material feeder 229 and line 231 to a similar but opposite gel material feeder 223, which supplies both relatively limited or smooth orifices or nozzles, as better explained in FIG. It will be included.

These devices also preferably include a support device to maintain the ribbon and direct the flow of gel material as it leaves the nozzle.

The pump 219 may be set to control the gel material loading rate, and by adjusting the charging speed of the spot, the spots of the required ratio may be continuously added to the fluid gel material. Preferably the pump 219 is the same as the pump 115 described above.

The gel material pressurizing device or extruder 229 and 233 and line 231 are preferably contained in a wall enclosed vessel 235, and are typically located in the center of the user, so that the gel material in the form of a sandwich with spots therein is contained in the vessel. And drop vertically or nearly vertically to the bottom of the center of these containers, from which product can be prepared via an outlet leading to line 237.

The outlet (not shown) is located at the bottom of the container, and the gel loading pad extends to the vicinity of the outlet, pulsating a ribbon sandwich containing spots that may cause air ingress (when vibration is not used). It is desirable to reduce rippling. It is also desirable to maintain the orientation so that the outlet shape matches the ribbon shape (usually square plane) and minimizes barriers to toothpaste release from the container and minimizes retention time, air incorporation and solubility of the spot binder. .

The spots added to the gelled toothpaste at the rates described above are contained in hoppa 230, preferably with a helix-type flow rate adjustable feeder 232, including a speed regulator and a motor combination device 234, the feeder being the Emitted through the outlet to the dispensing device 238 at the required adjusting speed, where the spot leaves the dispensing device, the spot forms a drop flow or thin curtain that matches the ribbon produced by the nozzles 229 and 233 in particle size and direction. It is desirable to do so.

Instead of helicar feeders, other feeders of screwed, belted and vibratory type may also be used. Line 228 is connected to a vacuum source, and line 259 may or may not be connected to the vacuum source.

Valves 239 and 241 are provided to arbitrarily select when the product is discharged via line 243 and when it is connected to pump 245, preferably of the Moyno type. The screw pump 245, driven by the motor 247, pumps the product through line 249 to a stationary bed mixer 251, preferably Kenic, which is gently blended and homogenized without disrupting, dissolving or dissolving the spots therein. Make a mixture. This is then conveyed via line 253 to receiver 255, which may be a supply tank for the tube filler, not described in this figure.

The apparatus of the present invention may be used without the use of a vacuum and the method of the present invention may be carried out. However, it is often preferred that no air is incorporated into the toothpaste material, and its vacuum or partial process may be under vacuum. Preferably the spot feeder and spot container should be under vacuum, so vacuum lines or taps 259 and 228 are shown in the figures.

In FIG. 5, gel material feeders 229 and 233 include nozzle sections 275 and 277 having planar tooling tools 263 and 265, respectively, limited to the nozzle part, which, as described, have adjustable support guides 267 and Each of the 269s are connected to set the proper orientation of the ribbon or webs of gel material so that the spot curtain or screen is positioned exactly above it.

The gel material on guide 267 is designated number 271 and is shown without spots attached. Similar ribbon 272 in guide 269 releases the gel material ribbon below the discharge location from the first guide and near the vessel outlet.

Preferably, the spot curtain falls vertically or nearly vertically on the ribbon 271 moving out of the ribbon's guide 267 but still with a horizontal moving component, such as 60 ° from horizontal. However, with care, it is possible to add spots on the gel material 271 while the ribbon is still in contact with the support.

As the gel material ribbon 271 falls vertically or nearly vertically with adhesive spots, it comes into contact with ribbon 272, and the two ribbons contain spots between them as sandwiches. In order to avoid the wave that causes air mixing, the guide 269 is preferably extended in a straight or conical curve shape to the vicinity of the exit hole (typically 5 to 25 cm) from the container so that the gel material ribbon is vibrated. It is a release rate that is equal to the sum of the angular velocities, without ripping, which is oriented and passes through a similarly shaped outlet.

The feed rate (and thickness) of the gel material ribbon may be approximately equal to the two, and may be changed as a relative speed usually in the range of 1: 4 to 4: 1. Adjusted and proportioned spots are conveyed from conveying tube 236 to dispensing device 238, shown in the form of expanding shutes, including sidewalls 279 and 281, bottom 283 and distribution pegs 285 located in the Pascal Triangle arrangement. do.

The openings around the spot and gel material feeder and the ejection nozzles of such a gel material feeder may be adjusted as described with reference to FIG.

The first or upper stream or ribbon of gel material should normally be oriented so that a spot flow or curtain of 0.5 to 5 mm thick can fall exactly on it, preferably the spot falls almost vertically and the gel material Moves in the horizontal component direction. This is where the gel material passes under, falls into, and sticks to the drop spots.

The ribbon 271 falls in the downward direction to the right, the spot 273 falls on the ribbon 271 from the distribution device 238 of the direction adjuster 235 (FIG. 4), and the ribbon 272 falls downwards from the bottom of the ribbon 271 to the left. It is shown.

The apparatus described in FIGS. 2 to 5 and the manufacturing method associated therewith provides a method for quickly and effectively preparing sparkling toothpaste without the need for further use of a conventional shear mixing device. In addition, the spots do not clump together or collapse, and because the preparation is rapid, the product can be filled quickly and filled into the tube before significant softening or dissolution of the toothpaste binder occurs. Thus, a preferred cotton gel toothpaste, which is an interesting dispersion of discretely visible discrete functional spots, is prepared in a state without any blurring caused by the destruction of toothpaste or the grinding of finely divided functional materials such as polishes.

Other advantages of the present invention include the non-fluidity of the spots on the gel material ribbon and the solubility of the binder used in the solvent material that may be present in the gel material.

By reducing the residence time in the device from the point of attachment of the gel material feed to the point of release of the gel material moving vertically to the vessel outlet, it reduces the dissolution of the spot binder and prevents the breakdown of the spot. . In addition, as described in FIGS. 4 and 5, the sandwich effect has a better bonsai effect in the dentifrice material of the spot, and in particular, it is possible to obtain an excellent effect in the toothpaste composition where the spot is not strongly adhered.

According to the wide range of manufacturing properties of the present invention, the preparation of toothpastes containing separated spots dispersed therein is in the form of gels or pastes which form the main component of toothpastes containing a gelling agent which facilitates the surface sticking to the spots. Preparing a flow of dentifrice composition; Preparing a spot flow to be dispersed in the toothpaste; Spray this spot flow onto the surface of the toothpaste composition; In addition, by adjusting the relative supply rate and flow rate of the toothpaste composition and the spots to be dispersed in the toothpaste, when the spot flow is in contact with the toothpaste composition flow, the spot is insufficient to cover the surface of the toothpaste composition, and the spot is the toothpaste composition. It consists of a step of adhering to, and in this way a toothpaste containing spots dispersed in the required ratio in the toothpaste is produced.

The device for advancing the above-mentioned manufacturing method is a normal toothpaste except for spots dispersed therein, and is composed of a device for moving and flowing a toothpaste composition flow having a property of spots sticking thereto. In such a device, by pushing the toothpaste composition through a suitable orifice, the toothpaste composition is extruded from the orifice into the desired shape, preferably in the form of a planar ribbon, to produce a gelled toothpaste stream or ribbon; A spot stream or curtain having a particle size within the range of US Si-B series 10-80 Si-B is applied to the gel-like ribbon so as to disperse onto the inside of the flowing gel-like ribbon surface and adhere to this ribbon; Further, the gel ribbons with spots on their surfaces are collected in a wall enclosed container, from which the gel ribbons with spots are continuously removed.

In a preferred embodiment of the present invention, the spots are added in the form of sandwiches between the toothpaste ribbons, and the spots are used to form a uniformly falling spot curtain by using a Pascal triangular barrier device.

The following examples illustrate the invention but do not limit the invention. All parts in the entire specification, including examples and claims, are by weight unless otherwise indicated.

EXAMPLE

5 parts ethylcellulose (10 cm poise) in powder form having the physical properties described in the preceding specification was dissolved in 5 parts ethanol (95%) and in a Hobert mixer having a particle size range of 0.5 to 10 microns or an average particle size range. It is mixed with 95 parts of predetermined alumina (Micrigit WCA 9F) of 3 to 5 microns. The mixing was continued for about 4 minutes until the blend was homogeneous, the mixture was pushed through 10 times (US-Si-based) screen and the extruded material was dried by drying at 65 ° C. for 1 hour. The dried agglomerates were then screened at screen 30 and collected dried speckles consisting of calcined alumina and ethylcellulose remaining on screen 60. The resulting spots are in poor form, with a ratio of maximum length / maximum width usually in the range 1-2, and most of the particles in the range 1.1-1.5. The angular shape of the particles may be a factor in the manufacture of toothpaste that is of interest to some consumers.

Transparent (or translucent) toothpaste base (all components except spots) may be prepared from the following ingredients.

After slowly combining 5 parts of the aforementioned spots with a particle size of -30 + 60 (US-Bev series) with 95 parts of the above-described toothpaste base agent in a slow moving mixer (about 2 rpm), the mixture was degassed and Automatically fill the tube and seal it. During the mixing, degassing and tube filling phases, spots that are almost uniformly dispersed in the toothpaste are more preferably stored for about one month when the tube is opened after filling by maintaining separation independence and insolubility in the toothpaste base. When squeezing the toothpaste through the outlet, the spots remained intact in contrast to the blue gelled material. If the product is evaluated without filling and immediately after filling, the spots are perceived as tactile, but if stored for a period of one year or more from two weeks prior to use, flavor oil, sometimes a dental detergent or other surface active agent may be present And with the help of other compositions, the ethyl cellulose is softened by dissolution so that the shape of the spot is sufficiently identified. It is in a state where it cannot feel the touch satisfactorily. While brushing with toothpaste, the spot particles are easily reduced in particle size, do not irritate the gums, and can be easily removed from the oral cavity when brushing is finished.

Although the presence of anionic detergents in toothpaste bases may play a supporting role, it is believed that the regulatory ingredients of such bases are 1.2% of the flavors present. Since it usually acts as a solvent of more than half of the ethyl cellulose of the flavoring agent, 0.5 to 2%, preferably 0.8 to 1.5% of a flavoring agent or a mixture thereof is preferable for the best spot dispersion, and the flavor is usually a dissolved hydrocarbon. And at least 50%, and often at least 80%, of esters, alcohols and aldehydes.

The described toothpaste manufacturing method in which the spots are dispersed in the body of the gel material should be monitored to ensure that the spots do not collapse, and that any indication of such signs should be stopped and usually unacceptably opaque. However, it is a recipe that must be filled immediately without causing serious adverse effects on the toothpaste appearance. Instead of using the mentioned mixing method, it is preferable to use other treatment methods already mentioned in the present specification, in which the spots controlled by this method are attached to gravity on a continuous drop extruded ribbon of gel material to which the spots adhere. To obtain a uniform spot dispersion in the toothpaste.

When the patched toothpaste of the present invention is packaged in an inelastic aluminum tube, the spots in the toothpaste cannot be observed until it is released from the tube. To give. However, when using flexible transparent tubes such as polyvinyl chloride or other suitable polymer tubes instead of conventional aluminum tubes, the spots can be seen through the tube and the clear gel-based toothpaste base, and even after squeezing the toothpaste, they can be observed. Can be. This in turn provides aesthetic benefits and makes children more interested in brushing, especially. Incidentally, functional spots act as a ventilator for people who use toothpaste that contains polishes or other functional ingredients of toothpaste, which reinvent the importance of brushing that such ingredients may be effective.

The above-mentioned ingredient is one gel gel toothpaste that can reduce the conventional 41.04% sorbitol solution to 36.04% and add 5% of spots. The reason for changing only the binary component is to maintain the concentration of the other toothpaste components except the sorbitol component as the main component at the same concentration as in the unignitioned product. When the spot density in such a toothpaste changes, it is judged that a component change can be continued in this way. However, starting from an initial gel material formulation, such as containing 41.04% sorbitol solution, it is also possible to proportionally reduce the proportion of each component to introduce the required amount of spots.

In one variation of the experiments described above, a 1% royal blue pigment may be used instead of 1% Microgit to make the spots blue. 0.5 to 2.0% of the same pigment or a 1:10 to 10: 1 ratio of pigment and brightener mixture may be used instead of the above-mentioned ratio of the royal pigment.

Alternatively, about 0.1 to 1% of a suitable water insoluble (or oil soluble) dye may be used. In such a case, the dye solution may be omitted from the dentifrice base component, and a dye solution may be added if sufficient distinction is possible between the spot and the base agent.

Of course, the various components of this structure may be replaced by other components as described above, and useful products are also obtained.

For example, other mentioned pigments and dyes may be used, and sodium lauryl sulfate may be substituted by sodium ethoxylated higher fatty alcohol alcohol sulfate or sodium halogenated coconut oil fatty acid monoglyceride monosulfate, and the brightener is dicalcium phosphate 2 It may be substituted with a hydrate and / or a dicalcium phosphate (anhydride) or a mixture thereof. The various component ratios may be modified by ± 10%, ± 20% to ± 30% as long as they are within the above-mentioned ranges, although the component ratio of the present embodiment is preferred, and at this time, satisfactory products having similar characteristics Can be obtained.

Example 2

75 parts of fine dicalcium phosphate and 15 parts of dicalcium phosphate dihydrate, both of which have an average maximum particle size of about 4 microns, are mixed with 10 parts of ethylcellulose and 10 parts of ethyl alcohol in a Hobert mixer. Alternatively, preferably, ethanol and ethylcellulose may be premixed, and then mixed with a pre-made dicalcium phosphate blend. The resulting material is pushed through a screen having a uniform opening of 2,000 microns and then dried at 65 ° C. for 1 hour on a drying furnace. The dried nodules are then sieved through a screen having a uniform opening of 420 microns and collecting nodules that do not pass through the screen with a uniform opening of 177 microns.

Subsequently, the obtained aggregated functional particles were replaced with sodium aluminosilicate, such as those marketed under the trade name Zeolite 4A in the toothpaste base, and the spot content in the final product was 2% (3% sorbitol solution content). Mixed with a toothpaste base agent of the ingredients given in Example 1.

As a polishing agent for spots in variations of this composition, hydrated alumina having an average particle size of less than about 10 microns, calcium carbonate having a particle size of about 7.4 microns or less, or an insoluble sodium metaphosphate having an average particle size of about 5 microns (all such particle sizes) May be final particle size).

The toothpaste of this embodiment is a semi-sparkling transparent or translucent product with an aesthetic appearance. Visible particles of flocculant varnishes (where other functionally insoluble substances may be wholly or partially substituted) are completely uniformly dispersed as a visual separation unit in the toothpaste base and rarely lose their form until use after 3 months storage.

Example 3

Instead of dissolving ethylcellulose in ethanol or other suitable solvent, a brightener and ethylcellulose, in some cases reduced ethanol, are added and combined to form a powder blend to form a nodule.

Such formulations are compressed in a rotary tablet compressor to produce slags about 6 mm thick and about 25 mm diameter. This slag is then granulated in a vibratory granulator, preferably made of small particles that pass through screen 30 and hang on screens 60 or 80. This method of making spots may also be applied to any of the spot components given in the previous examples. Although the binding effect of ethyl cellulose may not be large, the product of this embodiment may also be satisfactorily mixed in the toothpaste, contributing to the aesthetic and donor effects. If the binding effect of ethyl cellulose in the above-mentioned structure is not sufficient, the content thereof may be increased by 100 or 200% in some cases, but this increase incurs an additional cost, thus making ethyl cellulose or ethanol Wet methods using solutions dissolved in other suitable solvents are usually preferred.

Example 4

95 parts of calcined alumina (Micogit WCA 9F) having a particle size range of 0.5 to 10 microns and an average particle size range of 3 to 5 microns is a three-part powdered polyvinyl film commercially available from GAF Corp. as Plasdon K-29-32. Combine with Ralidone.

Two parts of ethylcellulose powder of the type mentioned in Example 1 are dissolved in 5 parts ethanol (95%) and the PVP-alumina blend is mixed with the solution in a Hobart mixer. After mixing is continued for about 4 minutes until the blend is uniform, the mixture is pushed through screen 10 and the extruded material is dried by drying as described in Example 1.

The dried nodules are then separated and collected as described in Example 1. The produced spots are rectangular in the maximum length / maximum width ratio as in the case of the first example. The transparent (or semi-transparent) toothpaste base (all components except for spots) was prepared in the same manner as in Example 1 except that a 39.04 part solution was used instead of a 36.04 part sorbitol solution.

After gently blending two parts of the aforementioned spots having a particle size of -30 + 60 (US particle size series) with 98 parts of the above-described toothpaste base agent in a slowly moving mixer (about 2 r.pm), the mixture is degassed and It is automatically filled in the flexible tube and then sealed. The process used is the same as described in Example 1. When assessed immediately after filling without storing the product, the spots have a tactile sensation, but if stored for two weeks to one year or more before use, the spots soften sufficiently and lose touch, which is due to the dissolution of PVP by the moisture present and This is due to the dissolution of the ethyl cellulose in flavor oils, and both dissolution reactions can be greatly increased with the aid of toothpaste detergents or other surface active agents, which in some cases may also be contained. do.

When the percentage of flavor in the gel-like toothpaste base is reduced to 0.6%, ie half of the above structure, the PVP-ethylcellulose binder system at the spot is still effective and maintains a satisfactory form during their storage.

This is also true if the flavor concentrations are changed to 0.3%, 0.9% and 1.5%. However, when the ratio of PVP and ethylcellulose is preferably the same as, for example, 2 parts PVP and 3 parts ethylcellulose, increasing the proportion of flavor (and / or other lipophilic solvent) is somewhat less than desirable. Dissolution proceeds quickly. Similarly, if the non-tactile properties of the spots need to be increased more than necessary, the spots can be softened further by increasing the PVP ratio, for example by doubling the ethyl cellulose.

The concentration and particle size of the spots can be varied within the ranges described above. In addition, the above-mentioned other substances may be substituted with alumina varnishes, including other types of water-insoluble functional substances. Modifications of the formulations and preparations described in Example 1 can also be made in this example, and the obtained products are also useful spots and ignition toothpastes.

Example 5

Both 75 parts anhydrous dicalcium phosphate and 15 parts dicalcium phosphate having an average final particle size of about 4 microns. The dihydrate is mixed with 5 parts ethylcellulose, 5 parts PVP and 10 parts ethyl alcohol in a Hobart mixer. Alternatively, preferably, ethanol and ethylcellulose can also be premixed and then mixed with a previously prepared blend of dicalcium phosphate and PVP. The resulting object is pushed through a screen having a uniform opening of 2,000 microns and then dried at 60 ° C. for 1 hour in a drying furnace. The dried nodules are then sieved through a screen having a uniform opening of 420 microns and collecting nodules that do not pass through the screen with a uniform opening of 177 microns. The agglomerated functional particles obtained are then mixed with the toothpaste base agent of the structure given in Example 4, except that the brightener in the toothpaste base agent is substituted with sodium alumino-silicide as marketed under the trade name Zeolite 4A.

The toothpaste of this embodiment is a semi-sparkling, transparent or translucent product and has an aesthetic appearance. Even in the case of modification of the structure and manufacturing method as in Example 2, an excellent product having the required properties is obtained.

Example 6

The functional brightener component of Example 5 was replaced with a mixture of anhydrous dicalcium phosphate and 90 parts of calcium carbonate, and the same amount of polish was used. Follow the same other procedures. The obtained product obtains a similar degree of satisfaction in functional effect and obtains aesthetic appearance in appearance. Similar results are obtained when the mixtures described above and other mixtures are replaced with in-spot containing mixtures and when this component is modified.

Example 7

Instead of dissolving ethyl cellulose and PVP in ethanol or other suitable solvents, a brightener, PVP and ethyl cellulose, in some cases, reduced weight ethanol is added and blended to produce a powdered blend as in Example 6. Obtain nodules. Such formulations are compressed in a rotary tablet compressor to produce slags of about 6 mm thickness and about 25 mm diameter. The slag is then granulated in an oscillating granulator, preferably made of small particles that pass through screen 40 and are hung on screen 60 or 80. The binding effect of PVP and ethyl cellulose may not be so great, but the product of this embodiment may also be satisfactorily mixed in the toothpaste, contributing to the aesthetic and functional effects.

In the above structure, if the binding effect of PVP and ethyl cellulose is not sufficient, the content thereof may be increased to 100 to 200% in some cases, but this increase incurs additional costs, and thus PVP and Wet methods using solutions in which ethylcellulose is dissolved in ethanol or other suitable solvent are usually preferred.

Example 8

In the previous example, polyvinyl pyrrolidone, the water-soluble binder portion of the mixed binder, was prepared by the following gum acacia, gelatin, corn starch, sodium carboxymethyl cellulose, sodium alginate, polyvinyl alcohol, horn star, xanthan gum and Complete or partial substitution (50%) with a water soluble binder such as gumtragacanth. When spotted on gelled toothpaste as described in the previous examples, this spot retains sufficient identity and integrity during the treatment process in the same manner as for spots prepared as PVP-ethyl cellulose mixed binders, but The toothpaste retains their original form but loses touch.

However, PVP-ethylcellulose mixtures are generally preferred in terms of their desired characteristics, including process stability, compatibility with toothpaste components, conversion of tactile properties to non-tactile properties without loss of appearance of spots or significant changes in appearance. It is generally judged to be excellent.

Example 9

Spots of various compositions were compared with spots based on ethylcellulose and PVP. The spot of the present invention is prepared according to the general method described in Example 4, that is, the wet method and the spot structure is the same as that used in Example 4, containing 95% calcined alumina, 2% ethylcellulose and 3% PVP. Spots of Comparative Experiment The wet method was also used except for one type modified using the wet or "slug" method of Example 7.

The spots were weighed 100 mg each for each type, placed on glass solvate, and 4 drops of water were added to each spot, and each slide was covered with another slide. It was done. When 2% sodium carboxymethyl cellulose is used as the binder, the spots lose their appearance within 15 seconds, and also in the case of spots combined with 2% hydroxypropyl methyl cellulose, in this case 2 It takes a minute. Spots prepared as a binder consisting of 2% methylcellulose and 3% PVP are softened through swelling. When the binder is 1% methylcellulose (400 centipoise), the spots lose their appearance after 5 minutes and when the binder is changed to 10% polyethylene glycol 6,000, the slug method with 1% magnesium stearate The spots produced by the eye lose their appearance after 15 minutes. The “control” spot of the present invention comprising 2% ethylcellulose and 3% PVP was stable even after 6 hours or more when subjected to the same test.

Example 10

In the production method of the present invention in which the apparatus of FIGS. 2 and 3 is used, semi-sparkling transparent gelling toothpaste is prepared according to the structure and method described in Example 1. The various gel (or paste) phase components are mixed together in mixer 111, and preferably transferred to an extruder having a relatively narrow square opening, ending with a flat "slit" nozzle, as described, with a Moyno pump. Preferably such nozzles are inclined at an angle of about 10 to 45 degrees, for example 30 degrees, downward from the horizontal.

The feed rate of the spot feeder, Acrisan Helix feeder, is controlled by the gel feed rate. Thus, for example, if a 3% spot content in a toothpaste is required, when the feed rate of the gel material is 3 kg / min, the spot is thus charged at a charging rate of 93 g / min. Conventional electronics or mechanical devices may be used to maintain the required charge ratio or to adjust if such changes in the ratio are required for other products.

In the drawings, the spot feeding mechanism is shown in FIG. 2 only as an explanatory view and in FIG. 3 only the purpose, but in a variety of types of feeders including screws, belts, basis weight belts and electrically controlled gravity feeders. Can be used and the release mode can also be changed.

There is very little release, but when the spot falls past the gel material, the gel phase flow can take on the impact spot. In addition, the spots fall apart and the gel material travels fast enough at the rate of 10 to 100 cm / sec, for example 20 to 50 cm / sec, so that each spot beats and adheres to the gel material. Few spots hit and bounce back with reaction. It also sticks to the toothpaste composition, which also constitutes all or almost all of these bounce spots.

Falling semi-ignition gels with spots attached to the gel material do not remain for so long in the vessel in which the anti-ignition device is located, falling through the center of the wall-enclosed vessel, with most of it going straight to the exit. . This short residence time in the ignition vessel is highly desirable, helping to maintain the integrity of the spots in the toothpaste.

Typical residence times are 20 seconds to 2 minutes with varying residence times in the vessel, but shorter times are better. This rapid passage, the absence of flow spots and the release of gel material from the center of the vessel also prevent the spots from agglomerating and becoming agglomerative masses. The additional volume of the side wall container is for retaining gelled material that can be supplied into the container for a period during which the stratification device may be temporarily stopped. The sidewall container may therefore contain only a small amount of semi-ignition gel, for example 10-25% of its volume. Alternatively, other materials in the container may act as a wall that binds the anti-ignition gel.

After passing through the ignition vessel, the gel material is pumped gently as a Moyno-type pump and thoroughly mixed through a fixed bed mixer. The Kenic mixer, which is a preferred stationary mixer, is the same as described in Handling Viscous Matericls-Materials Mixer for Viscous Polymer, published March 19, 1973, in Chemical Engineering.

Although it is desirable to use a mixer in the process prior to releasing the gel material into a filler or suitable storage container prior to use of such a machine, the present invention methods and apparatus are capable of sufficiently dispersing spots in the gel material without such a mixer. No mixer is used. Operating conditions are not an important issue, but usually 300-700 mm Hg vacuum, for example 400-600 mm Hg vacuum.

Temperatures are at or above room temperature, for example, 10 ° -40 ° C, and the release pressure of the gel varies with the degree of gel, but a pressure of 0.03-07 kg per square centimeter is good.

The various parts of the inventive equipment are used to make oral products and therefore must be made of non-corrosive and safe materials.

Mixers, emitters, pumps, tubes, and other parts that come into contact with liquid and gel materials are known to be made of stainless steel, as are the stainless steel components, which are quite good and used in the food industry.

When making 2% spot clear toothpaste (containing silicon dioxide, sorbitol, glycerol, CMC, sodium lysulfate, fragrance, water in the gel and alumina ethyl cellulose in the spot) as described in Example 1 A desirable product is obtained in which the spots are evenly distributed in the clear gel and are not stained or broken.

Similar results are obtained when making other spot toothpastes of known or of Examples 2-9 using the apparatus or process of the present invention as described.

In carrying out the process of the present invention, it is to be understood that the toothpaste gel or paste may be of a flat ribbon, but a variety of shapes such as arched ribbons or even cylindrical or tubular flows may be used.

It is also preferable to form a moderately thin and straight film such as 0.1 mm-1 cm or 1.5 mm-5 mm thick, while the spot flow or film may be dropped into gravity and enter the toothpaste directly. For example, in some cases, the flow of toothpaste moves vertically and the spots move horizontally against it, and the non-attached material is collected during recycling. The dental material stream can capture fully exposed surface spots that only move to one side by rotating.

The transported spot particles fill the gel stream and can be stored therein and separated without moving. However, the invention described and illustrated in spite of this operational variety is excellent.

The proportion of spots applied to the mobile ribbon or web of the gel toothpaste is small compared to the toothpaste containing the spots and the gel applied. The rate at which spots are applied is usually adjusted to such an extent that the amount of spots applied directly to the gel is insufficient to cover the gel, preferably not enough to cover more than half of the gel area exposed to the mucous membrane in contact with the gel. do.

On the other hand, it is preferable to drop the spot vertically on the membrane on the ribbon of the horizontally moving gel as described previously with other methods of attaching the spot to the gel ribbon. This direction has a horizontal or spotted gel that falls off and an important horizontal component, but normally it is preferred to tilt 10-60 ° horizontally for spots falling vertically after being released from the mobile device.

The viscosity of the gel, in which the spots adhere sufficiently to the gel, does not matter and the size of the particles does not matter, but is usually in the range of 10-80, preferably 30-80, and more preferably 30-60 sheaves. Is in. It is recommended that the spots be partially buried when the angle falls into the gel flow so that they do not move immediately, but similar results are obtained when round spots are used. Although it may be desirable to see the spots used in a transparent gel to make the product attractive, the spots have a refractive index that makes them invisible.

The spot is therefore preferably agglomerates of finely divided varnishes containing discrete particles, visible or absent of various materials. It is also preferable that the spot is a finely divided gloss agent or a flocculant of a binder while other active ingredients contain, for example, therapeutic agents, colorants, fragrances, fluorine and the like.

You should be aware that any toothpaste containing spots may be toothpaste except for spots, but not necessarily. Some toothpaste ingredients can be mixed with a number of other toothpaste substances. For example, it is desirable to apply some vacuum to the product before entering the kenics mixer but mix it with the fragrance containing some volatile components while the spot is stored.

This action prevents the loss of volatiles caused by the preservation of fragrance and the application of a vacuum during the speckling process and shortens the time for which the fragrance component that melts the spot's binder to contact them. However, it is possible to mix the flavor and toothpaste sufficiently by using a KENIX mixer or other relatively low shear stop mixers. Similarly, other ingredients are usually applied to the toothpaste after a small amount of auxiliary ingredient is added.

Sidewall containers falling on the spot toothpaste are either under vacuum or open to the atmosphere. The spot device has a reservoir beneath it rather than being in a container. However, such a device is preferably covered or under vacuum when air is a problem. This is not only a container for holding the product, but also applies as a container for the spot apparatus.

The process and apparatus are used to make different types of toothpaste containing different proportions of spots. Changing spot density is a simple matter. This is because the speed of the spot feeder can be changed and the gel feed rate can be adjusted accordingly. Some of the advantages of the present invention are increased operating efficiency, reduced use of moving part mixers, stabilization of toothpaste gels and pastes, and the like.

It has been found that several toothpastes are thinned by excessive mechanical work but by the present blend combinations that cause toothpaste to be spotted, such work can be avoided and the desired longitudinality of the toothpaste gel can be maintained.

Example 11

Although the process of making the sparkling toothpaste was performed in Example 10, the apparatus used was shown in Figs. Therefore, two half of each toothpaste (with few spots) was cut into two ribbons. The flat slit nozzle is tilted horizontally down about 30 °. The gel speed is about 20-50 cm per second and the gel is sufficiently adherent so that the conditions are well controlled so that most of the spots hitting the first gel stream are attached to the gel in a balanced manner with other gel streams.

As in Figure 5, the spot material falls into the nail in the Pascal triangle. It is tilted down about 30 ° horizontally and is about 90% of its width at the mobile end of the gel flow. The Pascal triangle is good, of course, but other feeders can be used.

The resulting toothpaste has the same benefits as in Example 10. In addition, the process apparatus of this embodiment is particularly suitable for keeping the spots aligned and evenly distributed on the gel toothpaste when the gel is not strongly attached. This prevents spots from popping out, prevents the loss of spots, and eliminates the need to regenerate and collect unattached spots. In addition, even for non-adhesive gels (or non-adhesive spots), the spot loss is minimized so that the composition and amount of spots can preferably be adjusted to the final product.

The invention has been described in various embodiments, but is not limited to this embodiment of the invention. It is because it is obvious that a person skilled in the art can use a substituent or equivalent without departing from the present invention.

Claims (6)

Water, humectants, gelling agents, detergents and flavoring agents which are the gelling base agent components of toothpaste; Polishing agent for toothpaste uniformly disperse | distributed to a base agent; Toothpaste consisting of visible functional spots, which are a nodule of a water-insoluble powdered functional substance dispersed in a toothpaste and a water-insoluble ethanol-soluble ethylcellulose binder. 2. The toothpaste of claim 1, wherein the toothpaste is in the form of a transparent or translucent gel with visible spots, wherein the spots comprise 0.1 to 10% of the toothpaste. The composition of claim 2, wherein 5-40% glycerol, 5-50% sorbitol, 5-30% water, 0.1-5% gelling agent, 0.5-5% toothpaste detergent, 0.5-2% flavor And 10 to 40% water insoluble toothpaste polish in a continuous phase, and having a particle size in the range of 10 to 80 in the US Si-B series, and in addition to dicalcium phosphate, tricalcium phosphate, insoluble sodium metaphosphate, alumina 75 to 98% toothpaste brightener in oxide or salt state selected from the group consisting of silica, magnesium carbonate, calcium carbonate, calcium pyrophosphate, bentonite and zirconium silicate and mixtures thereof, 2 to 20% ethylcellulose and 0.1 Toothpaste consisting of from 1% to 3% of a spot consisting of from 1% to 1% of a water insoluble colorant. The toothpaste of claim 1 wherein the visible functional spots dispersed in the toothpaste are the nods of the water insoluble powdered functional material and the mixture of the water insoluble ethanol soluble ethylcellulose binder and the water soluble binder. 5. The toothpaste of claim 4, wherein the spots comprise 0.1 to 10% of the toothpaste and the water-soluble binder is PVP and the spots therein are visible. 6-5% glycerol, 5-50% sorbitol, 5-30% water, 0.1-5% gelling agent, 0.5-5% toothpaste detergent, 0.5-2% flavor And 10 to 40% water insoluble toothpaste polish in a continuous phase, and having a particle size in the range of 10 to 80 in the US Si-B series, and in addition to dicalcium phosphate, tricalcium phosphate, insoluble sodium metaphosphate, alumina And toothpaste brighteners and ratio range from 80 to 98% of oxides or salts selected from the group consisting of silica, magnesium carbonate, calcium carbonate, calcium pyrophosphate, bentonite and zirconium silicate and mixtures thereof. A toothpaste comprising 1 to 3% of spots formed from 2 to 20% of a binder consisting of 1 ethylcellulose and PVP.

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