KR820000486B1 - Process for preparing therapeutic dentifrices in unlined container - Google Patents

Abstract

A manufg. method of therapeutic dentifrices in an unlined aluminum tube which causes no corrosion is described, said unlined aluminum tube contg. a toothpaste compn. comprising a fluoride therapeutic agent, a solid paste, a liq. phase, and a fluoride corrosion and staining preventing amt. of an alk. earth metal, said amt. being about 0.005 to 0.20 weight percent, and said alk. earth metal being provided as the reaction product of a water soluble alk. earth metal salt with amorphous silica.

Description

Method for manufacturing toothpaste that does not affect unplated containers

The present invention relates to a method of mixing an appropriate amount of alkaline earth metal ions in an unplated aluminum tube to prevent corrosion and staining by a therapeutic toothpaste such as toothpaste.

The present invention relates to toothpaste compositions and, in particular, toothpaste compositions, such as toothpastes containing therapeutic agents or varnishes and other ingredients, wherein the composition is filled in an unplated aluminum tube to prevent corrosion and staining when stored for long periods of time. In order to mix an appropriate amount of alkaline metal ions.

The types of toothpaste on the market can be broadly divided into the following two types.

Cosmetic

· Therapeutic

Cosmetic toothpaste is free of fluoride and whitens teeth and promotes shine. Therapeutic toothpaste, however, contains fluoride as a preventive of tooth decay.

Compositions of therapeutic toothpastes, such as toothpastes, usually contain fluoride therapeutics, such as tin fluoride, monofluorophosphate or derivatives thereof, and brighteners, wetting agents and other substances. Such compositions are commercially available filled in aluminum or plastic tubes. It is preferred to use aluminum tubes, but when they contain therapeutic fluorine compounds, they have been found to have contraindications between the inside of unplated aluminum tubes and one or more toothpaste compositions resulting in staining and other corrosive effects. Such incompatibility is manifested by gas generation, swelling corrosion of the tube and black stains on the inner surface of the unplated aluminum container. Therefore, when selling therapeutic toothpaste today, the method of plating aluminum tubes with plastic lacquer or other materials substantially increases the packaging and sales price of toothpaste.

Since unplated aluminum tubes are much more economical and lighter, many attempts have been made to solve this problem. For example, US Pat. Nos. 3,662,060 and 3,624,199 refer to compositions that solve the above problem. U.S. Patent No. 3,678,155 also describes that when the toothpaste contains α-alumina trihydrate as abrasive powder, monofluorophosphate ions prevent corrosion of unlacquered aluminum tubes. U.S. Patent No. 3,864,471 also mentions compositions containing a polishing agent containing monofluorophosphate and alkaline metal carbonates and insoluble alkali metal phosphates, alumina or mixtures thereof to minimize corrosion of unplated aluminum containers.

It is therefore an object of the present invention to overcome or reduce the problems of the prior art.

Another object of the present invention relates to a new toothpaste composition which does not stain or corrode the unplated tube, and a new abrasive powder which can be used therein, and also a method and packaging for producing a toothpaste composition which does not cause staining of the unplated tube. It is about a method.

The present invention also relates to a non-corrosive treatment toothpaste composition containing an appropriate amount of alkaline earth metal ions so that the composition can be sold in an unplated aluminum tube.

Other objects of the present invention will be detailed when describing the manufacturing method.

In order to satisfy the above object, a therapeutic toothpaste composition comprising about 0.005 to 0.20% by weight of an alkaline earth metal ion per 100 parts of a fluorine-containing therapeutic agent, a brightener, a liquid substance, and a toothpaste composition and an unplated aluminum tube To provide. There is also provided a novel gloss that supplies alkaline metal ions.

The present invention further provides a method of preventing the non-plated aluminum tube from corroding or staining by the toothpaste composition as described above.

As mentioned above, it was not possible to produce commercially useful products that could be packaged in unplated aluminum tubes because of contraindications to the aluminum tube face and the composition of the toothpaste composition, in particular fluoride. Efforts have been made to overcome such problems by the prior art, but the problem still remains. The present invention overcomes these problems in a commercially useful manner and provides fluoride-containing toothpastes or toothpaste compositions that can be filled and sold in unplated aluminum tubes.

It has been found that the problem of corrosion of non-plated aluminum tubes when formulating therapeutic toothpaste compositions according to the present invention can be solved by mixing an appropriate amount of alkaline earth metal in the toothpaste composition. Alkaline metals which are preferentially related to the present invention are particularly calcium but magnesium or strontium may also be used. Calcium is preferred because it is readily available, inexpensive, and easily blended into toothpaste. The metal may be mixed with the toothpaste or mixture in water-soluble form such as nitrate, hydroxide, oxide or chloride. Most preferably the substances that can be mixed in the therapeutic toothpaste composition of the present invention are calcium nitrate, calcium oxide, calcium hydroxide and calcium chloride. In addition, organic salts such as calcium acetate, calcium formate and the like may also be used. Corresponding strontium and magnesium salts may also be used.

The only condition for alkaline earth metal salts is that the solubility is so high that it should be possible to prevent corrosion without causing any safety issues in the composition.

Of course, in the prior literature, toothpastes and other toothpaste compositions containing significant amounts of calcium salts are described. For example, US Pat. No. 3,864,471 describes compositions containing 40 to 50% calcium carbonate. The issue describes compositions containing 20 to 75% calcium carbonate. Calcium carbonate, however, is largely insoluble and not effective in preventing corrosion of the tube. Therefore, a feature of the present invention is an appropriate amount of water-soluble alkaline earth metal ions mixed in the toothpaste composition. The amount of alkaline earth metal contained in the composition according to the invention should be sufficient to prevent corrosion but not enough to interfere with the fluoride activity of the toothpaste. The amount of alkaline earth metal to be contained to prevent corrosion should be at least 50 ppm or 0.005 weight percent, and not more than 2000 ppm or 0.2 weight percent in order not to interfere with fluoride activity. Therefore, the amount of alkaline earth metal that must be present should be 50 to 2000 parts or 0.005 to 0.2% by weight per million parts of toothpaste.

As mentioned above, alkaline earth metal ions can be mixed with toothpaste in the form of a water-soluble salt. However, methods of using alkaline earth ions in combination with silica and silicate types of abrasive powders or polishing agents are also within the scope of the present invention. A sufficient amount of amorphous precipitated silica can be mixed into the therapeutic composition to supply the required alkaline earth metals, such as calcium ions, to solve the problem of corrosion and staining. Such toothpaste-structured precipitated silica contains calcium ions, polishes or thickeners on the surface of precipitated silica abrasive powder.

Precipitated silica or silicon dioxide, structure-controlled for the above-mentioned toothpaste, is a novel product sold by J. M. Huber Corporation, and is filed by the present applicant who provides alkaline earth metal ions in the composition by treating with alkaline earth metal salts. Silicon dioxide products of the type described in US Pat. Nos. 3,960,586 and 3,928,541. The products described in this patent are precipitated silicic acid or silicon dioxide pigments prepared by acidifying alkali metal silicates such as sodium silicate and acids such as sulfuric acid in the presence of an electrolyte or salt such as sodium sulfate. Precipitated silicas from which the sulphate is required for the production process can be described as the sulphate solution product. After preparing and washing the wet cake-type precipitated silica, the slurry is reslurried in water and sufficient amount of alkali alkali metal ions such as calcium hydroxide, calcium oxide, calcium nitrate or calcium chloride can be supplied to the silica in an amount necessary to supply the alkali earth metal ions directly. To be treated. When the silica is reacted with alkaline earth metal, it is carried out by shaking at ambient temperature. The amount of alkaline earth metal ions incorporated is sufficient to provide the required amount of alkaline earth metal ions in the toothpaste but is related to the desired amount of alkaline earth metal ions incorporated directly in the toothpaste composition.

Therefore, the amorphous silica material is pretreated with a critical amount of alkaline earth metal material and then the desired amount is mixed into the toothpaste composition. Such silica compositions show good cleaning effects at RDA values of 200 to 400 (RDA-Grabenstetter et al, J. of Dental Research, 37, 1060, 1958).

The precipitated silicon dioxide of the present invention promotes 3 to 15 percent by weight of a water soluble alkali metal sulfate solution, preferably sodium sulfate, into the reactor, and an alkali metal silicate solution, preferably sodium silicate solution, into the reactor at a pH of about 8 to 10.4. Prepare to add. As a result of this reaction, pre-polymerization of alkali metal silicates occurs.

The silicate concentration of the water soluble sodium silicate solution is about 10-25 wt%, more preferably 18-22 wt%, with Na ₂ O 2.6 SiO ₂ composition being the best.

Then raise the temperature of the aqueous solution to about 66 ° to 83 ° C. (150 ° to 180 ° F.) and continue shaking to add an aqueous solution of a mine having a concentration of about 10 to 25% by weight within a substantially constant pH range of about 8.0 to 10.4. Acidify. Preferably, the mine and alkali metal silicate are added simultaneously, as described in Applicant's US Patent No. 3,960,586. Applicants of US Pat. Nos. 3,960,586 and 3,928,541 to Applicants are prepared for the preparation of basic precipitated silica or silicon dioxide. Sulfuric acid is preferred as the mine because it has the best results, but nitric acid, phosphoric acid, hydrochloric acid, carbonic acid and the like may also be used, as described in US Pat. No. 3,960,586 of the present application. The time for adding the alkali metal silicate or sulfuric acid to the reactor can be predetermined and is generally related to the difficulty of controlling the capacity of the reactor and the reactor capacity and the difficulty of controlling the temperature and shaking. After the addition is complete, the acidified acid is continuously added until the pH of the slurry falls below about 6.0, preferably until it is within the range of about 4.8 to 5.0. The resulting slurry is a precipitated silicon oxide contained in the reaction solvent.

After the pH falls below 6.0, the slurry-like material is heated to 10 to 30 minutes at 10 ° C to 30 ° C to warm up. The reaction temperature and the reaction pH mentioned above are adjusted if necessary. The resulting slurry-like material is filtered and washed with water to remove by-products such as sodium sulfate which may be contained in the silicon dioxide product.

In the course of the present invention, when the silicon dioxide wet cake is filtered and washed, alkaline earth metal ion treatment is used to produce the novel abrasive product of the present invention. According to the invention the wet washable filter cake is shaken at ambient temperature and slurried again in its own water or by addition of fresh water. When shaken, the slurry is treated with a sufficient amount of alkaline earth metal ions, preferably calcium ions, in the form of a dissolved salt to provide a sufficient amount of alkaline earth metal ions corresponding to 30 to 2000 ppm, which is closely related to silicon dioxide, 100 Based on wealth toothpaste. The amount of alkaline earth metal ions added is based on the total amount of anhydrides, which are recoverable solids contained in the wet cake form. Since the amount of polishing in the toothpaste composition can vary, the amount of alkaline earth metal salts also changes.

Alkaline metal ions are preferably used because calcium ions are readily available, economical, and easily mixed with silicon dioxide. Calcium ions can be mixed with silicon dioxide in water-soluble form, such as nitrates, oxides, hydroxides or chlorides, with lime oil or calcium hydroxide being preferred. Edible salts should also be used. Soluble salts may be used as long as they are soluble salts of calcium because only a very small amount of calcium ions need to be provided to the mixture. Organic salts such as calcium acetate and calcium formate can also be used. Corresponding strontium and magnesium salts of alkaline earth metals can also be used. The only limitation of the added alkaline earth metal salt is that it must be able to provide ions due to its high water solubility, which does not cause the safety problem of the toothpaste composition and must also provide the necessary fluoride.

After treatment with alkaline metal ions, the cake-like slurry material is vigorously shaken for 10-20 minutes, preferably 15 minutes, to provide sufficient alkali metal to the surface of the silicon dioxide, which is an abrasive. The product obtained is filtered and spray dried and pulverized according to known methods at an inlet temperature of 483 ° C. (900 ° F.) and an outlet temperature of 122 ° C. (250 ° F.) to a fine powder of the desired size.

Precipitated amorphous silica preferably used in the present invention has the following characteristics.

Oil absorption (cc / 100g Oil.Absorption-rub-Out Methol) 80 = 120

BET surface area (m ² / g) = 75-325

MSA Average Aggregate Size (microns) = 1-10

Bulk Density (lbs / cu.ft,) = 10-3

The present invention also includes other types of silica gloss containing Xerogel as described in US Pat. No. 3,538,230. Commercial xerogels such as Syroid 63 (Syloid 63, Davison Division of WR Groce & Co.) are mixed with an appropriate amount of calcium or alkaline metal ions or pretreated with calcium or alkaline metal ions as described above. Can be used when Therefore, sodium aluminosilicate brighteners can be formulated into the therapeutic compositions of the invention by mixing with critical amounts of alkaline earth metals as described in the specification.

As is known from the prior art, toothpastes, such as wetting agents and binders, are incorporated to enhance the texture and flowability of the toothpaste. Special formulations of toothpastes are known and are described, for example, in US Pat. Nos. 2,994,642 and 2,538,230 and in many patent publications. Further details are described in US Pat. No. 3,726,961.

Toothpaste formulations include pastes or dental creams which are very common from liquids and powders. Dental creams are more difficult to mix satisfactorily, as they must be balanced to produce a smooth and uniform paste, with care being taken to polishes, wetting agents, water, binders, preservatives, cleaning agents, fragrances, sweeteners and therapeutic agents.

Most toothpaste creams are polishes and use one of several common phosphates. Examples of phosphate brighteners include dicalcium phosphate anhydrous dicalcium phosphate, tricalcium phosphate, heat-modified dicalcium phosphate and insoluble sodium metaphosphate. The amount of phosphate added to dentifrices ranges from 5 percent to 60 percent by weight.

The most widely used humectants for toothpastes are glycerin and sorbitol. Propylene glycol is also used in small amounts and very limitedly. An important role of the humectant as part of the liquid agent is to maintain moisture to maintain a smooth luster when the paste is exposed to air.

The binder used prevents separation of liquid and solid phases. The most common binders are synthetic derivatives of seaweed colloids and celluloses, in particular Carrageenan and nitrile carboxymethylcellulose. Other rubbers have been used. Such a binder can also be mixed and used. Since natural and synthetic water dispersants of organic binders are invaded by microorganisms or fungi, relatively small amounts of preservatives are added to the paste. Examples of conventional preservatives are esters of parahydroxyl benzoate.

The cleaning agent's function in toothpaste formulations lowers the surface tension and foams in the mouth, increasing the cleaning action. The cleaning agents used are sodium N-laurylsarcosinate, sodium laurylsulfate, sulfoclaurate, sodium alkylsulfo acetate and sodium dioctyl sulfosuccinate.

Toothpaste fragrances are the single most important component of consumer preference, so care must be taken in choosing a balanced mixture of different essential oils. In rare cases, they may be used alone. Primary fragrance mixtures are green tea, peppermint and sasaffras and are used with ancillary oils such as pimento, cloves and anise.

Saccharin and sodium cyclate are used to improve paste and enhance the fragrance of toothpaste. The combination of synthetic sweeteners gives the best sweetness and no aftertaste. Their desirable properties appear even at low concentrations and have little effect on the toothpaste consistency.

Since water is used as a common urea, it is important to obtain a stable toothpaste using nearly pure water. It is common to use water without inorganic powder.

It is also within the scope of the present invention to provide an appropriate amount of alkaline earth metal in the dentifrice composition by pretreating the water with calcium or alkaline earth metal so that the water used can be provided as an alkaline earth metal source.

The present invention is applicable to any therapeutic formulation comprising alkali metal fluorides such as sodium fluoride, sodium monofluoro phosphate tin fluoride, and the like, which can be used in therapeutic toothpaste compositions.

Typically, such dentifrice compositions contain about 5 to 30 weight percent of a brightener, up to about 1 weight percent of fluoride containing therapeutic agents, and about 30 to 40 weight percent of deionized water, with the remainder being glycerin, sorbitol and other liquids. Carrier material. As mentioned above, according to the invention, the composition also contains from about 0.005 to 0.20 parts of alkaline earth metal ions, preferably calcium ions, based on the toothpaste composition. The amount of alkaline earth metal described above is sufficient to solve the problem of staining and corrosion of the unplated aluminum tube, but insufficient to interfere with the fluoride activity in the toothpaste and does not inhibit the therapeutic action of the toothpaste composition.

For mixing controlled amounts of alkaline earth metals in the compositions of the present invention, Degussa Technical Bulletin 49 describes "Aerosil 200" polishes which can be used in chalk toothpaste, page 8 of the document, which contains more economical polishes. The use of “aerosil 200” for choke toothpaste can prevent the use of less costly racker-clad aluminum tubes because the corrosion of uncoated aluminum tubes is suppressed by the production of small amounts of insoluble calcium silicate from the composition. It should be noted that it is described.

1% of "Aerosil 200" is the minimum requirement. However, the use of aerosils on page 8 of the same publication also states that corrosion protection of untreated aluminum tubes is not effective when the toothpaste composition contains fluoride in the form of monofluorosodium phosphate. However, it is described on page 5 of this document that corrosion of the light hydrated alumina W-16 to 3% by weight with a fluoride-containing toothpaste can be prevented. Contrary to this documentary technique, it was found that unplated aluminum tubes can also be used in accordance with the present invention if a suitable amount of alkaline earth ion is mixed with a fluoride-containing toothpaste.

When the silica type product is mixed with the toothpaste composition of the present invention, it can be considered that all silica products and raw materials contain trace amounts of calcium. For example, the presence of 0.01 percent calcium as calcium oxide is described in a commercial publication describing xerogel solids sold as Syroid (63).

This corresponds to 0.07 percent calcium or 70 ppm for Siroid 63. However, since only up to 35 weight percent of the silica product can be mixed in the toothpaste composition, this indicates that the originally produced toothpaste can contain only 0.0035 weight percent calcium oxide or 25 ppm calcium, which is not sufficient for corrosion protection. Do. Jay as described above. M Hoover. Since the precipitated silica of the corporation has a tendency to react with calcium ions, mixing with a controlled amount of calcium ions is interesting, and can also be incorporated into toothpaste because it imparts abrasive properties to the toothpaste composition.

The silica abrasive described herein uses about 15 to 30 weight percent of toothpaste. Thus, the abrasive must contain at least 168 ppm of calcium at 30 weight percent and 336 ppm of calcium at 15 weight percent to provide the minimum amount of calcium. However, it may also contain up to about 7000 ppm or more.

The following examples further illustrate, but do not limit, the nature of the invention. The composition is prepared by conventional methods and the amounts of the various components are by weight unless otherwise indicated. In the following examples and specification, parts are by weight unless otherwise indicated.

EXAMPLE

In the following examples a dentifrice composition is prepared and compared to a commercial raw or control product. To evaluate the toothpaste composition, use a graded chart on the inner wall of the tube to determine the presence of stains and corrosion. The composition is prepared based on the chart and then treated at 49 ° C. for 9 weeks. Data on the soluble fluoride ion percentage and tube mixing are determined periodically during the 9 week storage safety period. In this test, each three-week period under standing conditions (49 ° C) is equivalent to about one year at room temperature. The unplated tube containing the composition is periodically exposed during the experiment and stain and corrosion tests on the inner wall of the tube are made. The example in the following table is used to grade the composition properties in the tube.

In all the examples, the alkaline earth metal is calcium and the amount of calcium indicated in each composition is added in the form of soluble calcium nitrate.

Example 1-4

[Glossy Toothpaste Composition]

The following toothpaste composition is prepared with a low molecular weight silica polish and a known amount of calcium is added to the composition to have a tubular synthesis.

* Low molecular weight silica containing 5 ppm calcium.

** Conversion factor of calcium nitrate 4H ₂ O to calcium: 5.9 OaWO ₃ ) Molecular weight of ₂ · 4H ₂ O: 236

Atomic weight of calcium: 40 Therefore, 236 parts of calcium nitrate 4H ₂ O provides 40 parts of calcium ion, or 236/40 or 5.9 parts of calcium nitrate 4H ₂ O (corresponding to 1 part of calcium).

Calcium nitrate 4H ₂ O corresponding to an amount of calcium of 0.0295 / 5.9 or 50 ppm (0.005 percent), 100 ppm (0.01 percent) and 700 ppm (0.07 percent) in compositions 2, 3 and 4 is added to the dentifrice composition. Tube suitability data of this example are listed in Table 1 below.

TABLE 1

It can be seen from the above table that Composition 1 shows undesirable results in tube suitability testing because it does not contain a minimum threshold of calcium in the therapeutic toothpaste composition.

Example 5-8

The following toothpaste composition is prepared, in which each sodium monofluorophosphate content corresponds to 0.1 percent fluoride ion.

(A) Low molecular weight silica of composition 5 containing 5 ppm calcium

(B) Low molecular weight silica of composition 6 containing 168 ppm calcium

(C) low molecular weight silica of composition 7 containing 406 ppm calcium

(D) Low molecular weight silica of composition 8 containing 688 ppm calcium

The low molecular weight silica used in Examples 5, 6, 7, and 8 has the following characteristics.

Oil Absorption (cc / 100mg, Rub-Out Method) = 80-120

BET surface area (m ² / g) = 75 = 75-325

MSA Average Aggregate Size (microns) = 1-10

Bulk Density (lbs / cu.ft) = 10-30

Low molecular weight silica treated with calcium of compositions 5,6,7,8 is prepared according to the following preparation method:

Anhydrous sodium sulfate is added to 10.0 gallons of water in a 200-gallon reactor so that the concentration in the reaction solvent is 10 percent. The pH of the reaction solvent is adjusted to 9.0 by addition of sodium silicate. The reaction temperature is 65 ° C. (150 ° F.). The sodium silicate solution has a molar ratio of SiO ₂ , Na ₂ O of 2.5 and also has a concentration of 2.0 pounds per gallon. Sodium silicate is added to the reaction solvent for 4 minutes. The addition of sodium silicate is then stopped and the pH is adjusted to 9.0 by adding 11.4 percent sulfuric acid to the reaction solvent. Then, sodium silicate solution and sulfuric acid solution are added simultaneously for 35 minutes. After adding silicate for 35 minutes, the silicate is stopped and acid addition is continued to bring the pH of the slurry to 5.5. The batch is then immersed at 77 ° C. (170 ° F.) for 20 minutes and the resulting wet cake is recovered and washed.

The wet cake is divided into four parts and treated as follows.

Each batch of wet washable filter cake is reslurried without adding water while shaking at ambient temperature. During shaking, the slurry is treated with a sufficient amount of cortex-grade (US pure food grade) hydrated lime oil (calcium hydroxide) to bring the amount of calcium ions described in compositions 5,6,7,8.

The amount of calcium hydroxide is based on the weight of anhydrous solids that can be recovered in the form of a wet cake. After treatment with calcium ions, the cake-like slurry is vigorously shaken for 15 minutes to allow sufficient calcium ion treatment on the surface of the silicon dioxide abrasive. Each product is spray dried and ground at 483 ° C and 122 ° C for discharge.

Compositions 5,6,7,8 are left for 9 weeks at 49 ° C. and tube suitability data is periodically examined during the 9 week storage safety period. The results are described in Table 2 below.

TABLE 1-2

Toothpaste composition 5 in the above table, it can be seen that when left for 9 weeks, very severe black stains and scratches on the tube wall. Compositions 6, 7, and 8 are stable and show good tube fit. As such, it can be clearly seen that the silica polish does not corrode the unplated aluminum tube if it contains the minimum threshold of calcium.

Example 9-11

[Stabilization of Toothpaste for Xerogel Therapy by Calcium]

Therapeutic toothpaste is prepared with a xerogel polish. All compositions (except composition 9) contain a known amount of calcium ions (added with water-soluble calcium nitrate). The composition is prepared according to conventional methods and filled in an unplated aluminum tube. Amount indications of various components are by weight unless otherwise indicated.

Toothpaste compositions are prepared as follows. Each sodium monofluorophosphate content corresponds to 0.1 percent fluoride ions.

0.18 percent and 0.30 percent calcium nitrate.4H ₂ O in compositions 10,11 correspond to 0.18 / 5.9 or 0.03 percent calcium (300 ppm calcium) and 0.30 / 5.9 or 0.5 percent calcium (500 ppm calcium).

From the table, it can be seen that the composition of Example 9 does not contain calcium. The toothpaste of the tube is left standing at 49 ° C. for 9 weeks and then graded to determine 1,3,6,9 weeks.

Table 3 shows the degree of corrosion or staining of unplated aluminum tubes.

TABLE 3

It can be seen from Table 3 that the compositions of Examples 10 and 11 exhibit excellent tube suitability. It should be noted that a rating of 10 means unchanged in an unplated tube vessel. Since composition 9 does not contain critical amounts of calcium, undesirable results are obtained in a tube suitability test after storage at 49 ° C. for 9 weeks.

According to the supplier report, Xerogel and Syroid 63 have the following characteristics.

In addition to the above properties, Syroid 63 has the following chemical composition (supplier report);

Example 12

[Influence of Calcium on Commercial Toothpaste]

Fill the plated container with a toothpaste of therapeutic “Aim” clear gel to prevent corrosion and staining. “Colgate Dental Cream (CDC)” is also filled in the plating vessel.

In order to test the effectiveness of the calcium addition in solving the tube fit problem, “Aim” and “CDC” are purchased on the market and each is divided into subdivisions.

The “Aim” toothpaste is divided into A, B, and C, and the A part is filled into an unplated aluminum tube without adding calcium. Part B and C are mixed with known calcium and filled in unplated aluminum tube.

“CDC” (Colgate Dental Cream) is also divided into D, E and F, filling the D part with an unplated aluminum tube without adding calcium. A known amount of calcium is added to E and F. Data from “Aim” and “CDC” compositions in unplated containers are described in Table 4 below, with each composition as follows.

Example 12

TABLE 4

Compositions B, C, E and F have superior tube suitability compared to compositions A and D. Adding calcium helps stabilize the composition of therapeutic toothpaste.

Example 13-17

The following toothpaste compositions are prepared to illustrate the use of sodium alumino-silicon (SAS) as a brightener. The composition of Example 13 is used as a control without adding calcium. Known amounts of calcium are added to the compositions of Examples 13,15,16,17. The composition is as follows.

0.2% calcium nitrate 4H ₂ O in composition 14,15,16 corresponds to 0.0% calcium ion and 0.24% calcium nitrate 4H ₂ O in composition 17 corresponds to 0.04% calcium ion.

(A) The SiO ₂ / Al ₂ O ₃ ratio of the SAS product used in the compositions 13,14 is 11.0.

(B) The SiO ₂ / Al ₂ O ₃ ratio of the SAS product used in composition 15 is 2.5.

(C) The SiO ₂ / Al ₂ O ₃ ratio of the SAS product used in composition 16 is 130.

(D) The SiO ₂ / Al ₂ O ₃ ratio of the SAS product used in composition 17 is 400.

Preferred sodium aluminosilicate (SAS) has the following chemical composition.

xNa ₂ O · y Al ₂ O ₃ · z SiO ₂ · w H ₂ O where X represents the number of moles of Na ₂ O

y represents the number of moles of Al ₂ O ₃

z represents the number of moles of SiO ₂

w represents the number of moles of water.

When fixing y to 1, the value of z is the mole ratio of silica / alumina of SAS. The silica / alumina ratio or z value of the low molecular weight SAS abrasive and the polishing agent is 2.5 to 400.

The characteristics of the SAS varnish are as follows.

Oil Absorption (Rub-Out Method cc / 100g) = 75-125

BET surface area (m ² / g) = 50-300

MSA Average Aggregate Size (microns) = 1-10

Volume Density (lbs / cuft) = 12-35

Compositions 13-17 were left at 9O < 0 > C for 9 weeks, and tube suitability was evaluated after 1,3,6,9 weeks and the results are shown in Table 5 below.

TABLE 5

It can be seen from the above table that Compositions 14-17 exhibit good tube fit.

Claims (1)

A fluoride-containing toothpaste composition is mixed with 0.005 to 0.20% by weight of a water-soluble alkaline earth metal compound to prevent corrosion and staining due to fluoride of an aluminum tube that is not plated after prolonged contact with the fluoride-containing toothpaste composition. Method of manufacturing toothpaste.