JPS6386799A - Denture purifying and/or cleaning composition containing bleaching activator - Google Patents

Abstract

(57) [Abstract] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates generally to cleaning compositions, and more particularly to cleaning compositions in tablet form for use in denture cleaning and cleaning.

Cleanser compositions, especially hard surface cleaning compositions, use oxidizing and bleaching agents to remove visible dirt and at the same time have the ability to remove oxides and plaque that have formed on the optical surfaces to be cleaned. are doing. That is, mild cleaning compositions are known, including those prepared containing abrasive substances for use as a, i, p-9 cleansers, and those prepared containing abrasive substances in a liquid medium such as water. Some are formulated without abrasives for the purpose of gentle dispersion and surface cleaning, such as those formulated for immersion use, such as those of Yin-N detergents. All of these compositions use common sulfate salts, i.e., pisulfate, monopersulfate and sulfate, oxidizing agents, etc. as detergents, and also alkali metal dust and alkaline earth metal halides as bleaching agents. are doing.

Such compositions also generally contain perborates, carbonates, and phosphates in varying amounts to provide effervescence and activation. A representative cleaning agent composition covering these uses is disclosed in U.S. Patent No. 5.33 of Puetzer et al.
Otsu No. 466, U.S. Patent No. 5,704,227 to Hllll
No. 4,362,639 to Eoga and Eoga U.S. Pat.
No. 4,409,118, all of which are incorporated herein by reference.

If the cleaning compositions described above contain one or more borates and the compositions are prepared into compressible tablets, the formulation of one composition may be compressed to form a compressible tablet. The tablets have a particular drawback that they do not have mechanical strength.

These problems are mainly due to the physical properties of the perborate used. In particular, anhydrous sodium perborate has a small specific gravity and density, so it is commercially available as a fluffy powder that does not sag when compressed or agglomerated. The same difficulties, although to a much lesser degree, exist with the other perborate additive, sodium perborate monohydrate.

In the past, various attempts have been made to correct this drawback. For example, some of the prior art are standard tablets, such as Merck's Sodium Benzoate. It is intended to be added in an amount equal to the amount of motion aid for the product. However, the addition of these ingredients in large quantities alleviates the difficulties of initial processing and tablet forming;
Other disadvantages arise, namely, the delayed action of the formed tablet upon use, which is commercially undesirable. In particular, as the amount of tabletting aid increases, the disintegration time of the tablet increases, resulting in delayed tablet action and, in some cases, reduced dryness, reducing its appeal to potential consumers. do.

Br1chard et al. US ff14G 4,115,51
No. 9 is a sodium hydroxide solution that enables the preparation of monohydrate vJ granules of desired particle size, specific gravity, abrasion resistance, and flowability for use in connection with dental cleaning tablet compositions. A method for preparing borate monohydrate is disclosed. This technique was complex and expensive, requiring special equipment to perform fluidized bed particle formation with hydrogen peroxide.Hotko, U.S. Pat. It is disclosed that polyfluorocarbons may be used as lubricants in tablet manufacturing, with a weight range of about 1 to about 15% compared to known lubricants such as polyethylene glycols and the like. It is stated herein that the fluoropolymer may be added directly to the tableting mixture in its acceptable amount and amount as a lubricant, resulting in favorable effects in the tablet molding process.

HOtko's disclosure includes fluoropolymer and agglomerating agents.
There is no mention that 1, , acts as an auxiliary agent in the compressible composition and facilitates the production of a granulated material having an increased and preferred specific gravity.

No. 4,362,639 attempts to produce a cleanser with improved odor and discoloration resistance. Cleansers contain as ingredients oxidizing agents such as monopersulfate salts, halide bleach accelerators such as alkali gold or alkaline earth metals, effervescent compounds such as perborates, and salts. Ammonium ion donor is used to suppress the occurrence of bad odor and taste.

U.S. Pat. No. 4,405,486 discloses a method for preparing granulated saline which can be successfully used in black striped compositions, such as those formed into denture cleaning tablets. The method includes forming a mixture of one or more perborates and a polymeric fluorocarbon. The prepared particles have improved hardness and specific gravity, enhancing their role in compressed detergent compositions, as well as enhancing the disintegration properties of the detergent tablets.

Further, US Pat. No. 4,409,118 discloses the formation of tablets with good mechanical strength and excellent dissolution rate and purifying effect. By adding a polymeric fluorocarbon to the granulated compression preformed nonaperborate mixture, an improved composition is obtained that has no tendency to stick to tableting equipment and is dimensionally stable.

Also, U.S. Pat. No. 4,518,520 discloses that 4? KJL, discloses the preparation of cleaning compositions that have improved solution clarity and rapid dissolution rates when dissolved in water. In particular, these cleaning H formulations contain phosphate mixtures, anhydrous perborate salts and perborate monohydrate, the combination of which includes improved perborate formulations that include a polymeric fluorocarbon moiety. Contains a mixture of acid salts.

A-tooth cleaners and cleaning compositions containing bleaching activators are also known. See, eg, US Pat. No. 4,422,950. These bleach activators typically react with peroxides such as perborates in aqueous bleaching solutions to produce r! 9
．． It contains carbonaceous derivatives which form dissipates and increase the active oxygen content even at lower washing temperatures than K, thereby enhancing the bleaching action of the mixture.

To improve the shelf life of such bleach activator-containing compositions, the bleach activator is generally used in the form of a granulated cellulose, which requires the use of a binder material. However, these binders prevent the rapid dissolution of the granules when placed in the cleaning medium and, in some cases, tend to settle in the cleaning medium and remain substantially inert during the cleaning or cleaning operation. For bleach activators, the non-reactive bleach activators can be 50 or more. As a result, the production of peroxides is reduced and therefore the bleaching effect is also reduced.

Thus, the nature of the binder material affects the amount of peroxide produced. Most binders require water as a means of applying the binder material. Any amount of water
This causes premature decay of decomposed compounds, and also has an adverse effect on the long-term storage stability of the grains.

Thus, it has surprisingly been found that improved cleaners and cleaning compositions can be provided by incorporating improved bleach activator granules. The improved bleach activator granules of the present invention for use in cleaning and/or cleaning compositions include (1) a bleach activator; (11) an alkali metal perborate anhydride; and /
Makuwa OiD perphosate monohydrate of a metal selected from the group consisting of alkali metals, alkaline earth metals and mixtures thereof; and θ■) a polymeric fluorocarbon binder inert to bleach activators; Contains.

Further, by incorporating the improved bleach activator granules, effervescent cleaning and/or cleaning compositions in tablet or powder form are provided.

A typical cleaning and/or cleaning composition is as follows: (1) Based on the final composition, monopersulfate (mono-p
eraulfate 5olt) approx. 20 to approx.'s o
weight 1k % p(11) bleach activator; GiD anhydrous alkali metal perborate; and/or θφ perborate of a metal selected from the group consisting of alkali metals, alkaline earth metals and mixtures thereof 1 and a polymeric fluorocarbon binder which is inert to the bleach activator, and at least a portion of the bleach activator and anhydrous perborate and/or perborate monohydrate; A fluorocarbon binder is present in the compacted granule mixture.

The improved bleach activator of the present invention contains a bleach activator compound that reacts with decompounds to produce acid peroxides. Typical bleach activators are carboxylic acid anhydrides, carboxylic acid esters and N-acyl or O-acyl substituted amides or amines. Such bleach activators are for example A1
Deterge from 1enH, Gikbert IIC
nt Age 18-20 (June 1967),
30-66 - Ji (July 1957) and 26.27
and 6 Fiji (August 1957), all of which are incorporated by reference. The following is a representative but non-exclusive list of active agents for use in the present invention.

(a) N-cya heptatylated and N,N'-tetraacetylated amines, such as N,N,N',N'-tetraacetylmethylenediamine or monoethylenediamine/,N
, N-diacetylaniline and N,N-diacetyl-
p-) Luidine is a 1,3-diacylated hydantoin, such as 1,5-diacetyl-5,5-dimethylhydantoin and 1,3-dipropionylhydantoin; (b) N-alkyl-N-sulfonyl-carbonamide , for example N-methyl-N-mesyl-acetamide,
N-methyl-N-mesylbenzamide, N-methyl-N
-mesyl-p-nitro(nzamide, and N-methyl-N-mesyl-p-methoxybenzamide; (c) N-acylated cyclic hydrazides, acylated triazoles or diazoles, such as monoacetylmaleic hydrazide; (d ) O,N,N-)-substituted hydroxylamine,
For example O-benzoyl-N, N-succinylhydroxylamine, 0-acedel-N, N-succinyl-hydroxylamine, op-methoxybenzoyl, N,
N-succinyl-hydroxylamine, 0-p-nitrobenzoyl N, N-succinyl-hydroxylamine and O,N,N-)lyacetyl-hydroxylamine; (e) N,N'-diasilosulfurylamide, e.g. N, N'-dimethyl-N,N'-diacetylsul7lylamide and N,N'-diethyl-N,N
'-dipropionyl sulfur 7-lylamide; (f) triadyl cyanurates, such as doriacetyltaanurate and tribenzoyl cyanurate; (stirrup) carboxylic anhydrides, such as benzoic anhydride, m-chlorotetrabenzoic anhydride, 7-talic acid, and 4-chloro 7-talic anhydride: (→ sugar ester, e.g. LIdf glucose [11 ester; (i) 1,3-diacyl-4,5-diacyloxy-imidazolidine, e.g. 1,3-diformyl -4,5
CJ) Tetraacetylglycoluril and Tetrapropionylglycoluril; (Sec. Diacylated 2,5-diketobibenzine, e.g. 1
．． 4-Diacetyl-2,5-diketopi is radine, 1.4
-dibrobionyl-2,5-diketopiperazine and 1
．． 4-dipropionyl-3,6-dimethyl-2,5-diketopiperazine; (1) Acylated products of propylene diurea and 2,2-dimethylpropylene diurea, especially tetraacetyl or tetrapropionyl propylene diurea and their dimethyl derivatives; (where carboxylic acid esters, such as 1)-(ethoxycarbonyloxy)-benzoic acid sodium and p-(propoxycarbonyloxy)-sodium benzenesulfonate; and (n) alpha-acyloxy-(N,N')polyacylmalonamides, such as al7 Aacetoxy (
N,N')-diacetylmalonamide.

N,N,N',N'-Natho2acetylethylenediamine (ITA) is the preferred cleanliness activator of the present invention.

For purposes of this invention, the amount of bleach activator used generally ranges from about 10 to about 50 bags of granules, preferably a total of
The amount is approximately 25-35 liters by weight.

perborate (pe) used in the bleach activator granules of the present invention.
rborate 5alt) may be selected from alkali metal perborate and alkaline earth metal perborate;
It may especially be selected from alkali metal and/or alkaline earth metal perborate monohydrates and anhydrous alkali metal perborate salts.

Thus, sodium and potassium salts of perboric acid monohydrate and anhydrous perborate may be used, but preferably the perborate salts include sodium perborate monohydrate and anhydrous sodium perborate.

Also, heptammonium monohydrate or anhydrous perborate,
Also included are calcium and magnesium.

The anhydrous perborate salt is generally about 5 to about 50 parts by weight, preferably about 10 to 30 parts by weight, based on the total weight of the bleaching activator granules.
Used in an amount of ii%. On the other hand, perborate monohydrate is about 50 to about 601 ft based on the total weight of the bleach activator granules.
%, preferably from about 40 to about 5 Dii%.

The perborate salt component functions in the f1 capacity of the present invention, has a cleaning action, also promotes the activity of the composition by producing foaming properties, and further enhances the activity of the composition by producing foaming properties. This prevents discoloration and corrosion of easily damaged supports.

Another feature of the improved bleach activator of the present invention is the use of a binder material, namely a polymeric fluorocarbon. The polymeric fluorocarbons may be selected from the known classes of carbon and fluorine polymers and copolymers, which may further contain hydrogen and/or chlorine. Fluorocarbons can include at least one heptafluorinated olefin, including, for example, polytetrafluoroethylene, copolymers of tetrafluoroethylene and hexafluoropropylene, and vinylidene heptafluoride and hexafluoropropylene. Preferred polymeric fluorocarbons include polytetrafluoroethylene.

According to the present invention, the polymeric fluorocarbon binder used in the bleach activator granules is from about 101 to about 1Xfk, preferably 0.0
Used in amounts ranging from 5 to about 1718%. The fluorocarbon polymer may be used in the form of a powder having an acceptable particle size in combination with perborate and bleach activator, preferably in the range of up to about 150ξ. The exact particle size may vary, and average diameters from about 25 to about 75 microns may be used.

The particle size of the polymeric fluorocarbon is not critical to the practice of this invention.

Pentapolymer fluorocarbons such as polytetraethylene,
When the combination of perborate mixture and bleach activator compound is used in a foaming detergent powder or granules, or in the formulation of denture cleaning tablets or powders, the bleach activator compound is added in a clear solution. Allows the formation of compact, compact, hard granules such that the compound dissolves quickly.

By using a polymeric fluorocarbon such as polytetrafluoroether, it contains salt as an essential foaming component, is inert to bleach activators, and is therefore easily cleaned in cleaning media. In the grains that are dispersed in
Gives strength.

Polytetrafluoroethylene is preferred as K, binder and solidifying agent since it does not clearly reduce the dissolution rate of m-grains. That is, the composition provides a bleach activator compound with an effective acid peroxide that improves bleaching and cleaning. Further, in an aqueous medium, the preferred bleach activator granules provide a voice ranging from about 10 to about 115.

According to another embodiment of the invention, the improved cleaning composition comprises a monopersulfate, such as an alkali metal salt, typically potassium monopersulfate, preferably in tablet form. It is present in an amount of about 20 to about 60%, preferably about 50 to about 50% by weight of the total cleaning composition. The cleaning composition also typically contains about 5% to about 15% by weight of the total composition.
of phosphate, including the bleach activator granules described above. Preferably, the phosphate is about 8 to about 12
Alkali metal phosphates and/or alkaline earth metal phosphates may be present in amounts ranging from 1 to 1, with alkali metal phosphates being preferred. More particularly, the preferred alkali metal phosphate is sodium tripolyphosphate.

The phosphoric acid component acts as a cleaning agent. When the composition of the present invention is used as a denture cleaning agent, the phosphoric acid compound attacks and decomposes dental plaque that has formed on the surface of the denture. In addition to its function as a bilgu, phosphates also serve as such a cleaning agent.

In addition to the ingredients listed above, the cleaning and/or cleaning compositions of the present invention may contain various additional ingredients selected based on the end use. Thus, for example, the compositions may contain detergent compositions such as organic or inorganic detergents, including various polyoxyethylene ethers of aromatic and aliphatic alcohols and polyoxyethylene ethers of hydrophobic propylenoxide polymers. It also includes nonionic detergents such as. These compounds contribute to maintaining foam-forming action in aqueous solutions.

An example of a preferred detergent is sodium lauryl sulfoacetate, such as that available under the product name Lanthanol LAL. A suitable i for such detergents is from about 0.5 to about 0.9% by weight of total acids, with about 0.5% to about 0.9% by weight of total acids.
6 to about 0.8% by weight is preferred.

The compositions may also contain other auxiliary substances, which may be inorganic or organic in structure. That is, inorganic water-soluble alkali builders such as alkali and alkaline earth metal carbonates, hydroxides, and mixtures thereof may be added. In particular, sodium carbonate may be present in amounts of up to about 20 i% by weight, since its function is not only as a bilge, but also to enhance effervescence and to help stabilize the mass of the solution formed from the composition.

The compositions of the present invention may also contain sequestrants or chelating agents for the purpose of maintaining solution clarity when the composition is placed in solution. Metal ion sealants or chelating agents can also assist in inhibiting corrosion and rust in articles immersed in solutions containing the compositions of the present invention.

A useful sequestering agent is ethylene diamine diamine vinegar f
fi (ED'!'A) and its corresponding alkali salts, as well as other polyfunctional organic acids such as citric acid, maleic acid and their salts.

The sequestering agent may be present in an amount of about 2 to about 6%, preferably 6 to about 5% by weight of the total acid group.

v4!8 for use of the composition as a denture cleaner!
Flavors in varying amounts as described above, if desired.
Colorants, flavors, etc. may be added; for example, flavors include various mints, clove oil, artificial vanilla flavors, and others. These materials may be included and mixed in various combinations within the scope of the invention. Selection of the required amount is within the knowledge of the manufacturer.

When the cleaning composition of the present invention is formulated as a cleaning agent, the colorants used are F, D, &C.

&C, dyes and lakes are well known. These substances have been classified by the Federal Food and Drug Administration as
Approved for drug and cosmetic uses and as a drug and cosmetic colorant. The substances that are permissible for the abovementioned range of uses are F.

D, &C, known as Proof Super 2, includes an indigoid dye that is the disodium salt of 5,5'-indigothene-disulfonic acid. Similarly F, D.

&C, the dye known as Green Bian 2 contains triphenylmethane dye and is 4-(4-(Nz-thyl-p-sulfobenzylamino)-di7-enzymedelene)-(1-
(N-ethyl-N-p-sulfoniumbenzyl)-Δ2
#5-Cyclohequinadimine] monosodium salt. All F.

D, &C, Tori, &C, and the corresponding chemical structure i
j Kirk-Othmar Encyclopedia
a of Chemical Technology Y+
ti 3rd edition, 6@, 561-595, is described in -ji, this text is incorporated herein by reference. Dyes and colorants fade at different rates and may be selected to achieve a particular endpoint.

The colorants mentioned above may be mixed with each other in various combinations. It is particularly preferable to select a colorant that exhibits a deep color when the composition is initially dissolved. This means that
When the composition is used as a denture cleaning agent, it is important that the discoloration phenomenon inherent in the denture cleaning agent is easily observed by the end user.

The present invention further relates to dry mixing of % anhydrous sodium perborate, sodium perborate monohydrate, bleach activator and polytetrafluoroethylene and in a mobile granulation device or fitZmill. v4 of bleach activator granules, including direct sizing compaction using other known sizing techniques or methods! ! ! Including methods. The resulting granules generally have a particle size of about 10 to about 100 meshes, preferably about 12 to 30 meshes.

According to the present invention, the composition may be made into tablet form Kv4 without the need for increased addition of ingredients such as excipients, tabletting agents, etc.

Even when such components are added, the amount of these components may be reduced due to the favorable effect of the polymeric fluorocarbon in the compacted granules of perborate. Naturally, the minor additions of the ingredients will depend on their specific purpose, such as lubrication, but these additions and their respective amounts are not critical and are not part of the invention.

As mentioned above, improved cleaning and cleaning compositions can be obtained by incorporating improved bleaching agent granules. Although it is preferred to use the bleaching activators described, effective denture cleaning and/or cleaning compositions are prepared by incorporating a free bleaching activator into the composition, i.e. bleaching activator F! It is not first formed into a granulated mixture (granules) with the perborate, but rather is added as a separate ingredient into the composition. Such compositions provide another aspect of the invention, which is discussed below. Those skilled in the art will appreciate that, unless otherwise specified, the descriptions of various aspects and composition components containing a bleach activator can also be applied to the compositions described below that do not contain a bleach activator.

Thus, in another aspect, the present invention provides monopersulfates, anhydrous perborates and/or perborate monohydrates, polymeric fluorocarbons, bleaching activators, and optionally denture cleaning agents. Provided are improved effervescent cleaning and/or cleaning compositions in tablet or powder form containing known additives contained in the present invention. Typically, the following: (1) from about 20 to about 60% by weight monopersulfate, based on the final composition; (11) an effective amount of an anti-spreading agent; (]iD an effective amount of anhydrous alkali gold F! 4 perborate; and/or q■) an effective amount of a perborate monohydrate of a metal selected from the group consisting of alkali metals, alkaline earth metals, and mixtures thereof; and (V) an effective amount a polymeric fluorocarbon binder that is inert to a bleach activator, wherein at least a portion of the bleach activator and anhydrous perborate and/or perborate monohydrate and the polymeric fluorocarbon binder are compressed. An improved foaming cleaning composition is provided in a granular mixture.

It will be appreciated by those skilled in the art that the compositions of the present invention can be used in powder and tablet form. The composition that is ultimately compressed into tablets typically has an effective amount of polymeric 70 orocarbon in addition to the polymeric fluorocarbon binder present in the compressed granulation mixture. Generally, from about 0.05 to about 0.2. ii is used, but approximately Q, 0
9 to about O/12 full weight is preferred. The composition may optionally contain effective amounts of other known additives, i.e. phosphates, detergents,
Inorganic water-soluble alkali builder auxiliary substances, chelating agents or sequestering agents, flavors, colorants (dyes), fragrances, excipients, fillers such as sodium sulfate, benzoic acid Contains things like more preservatives such as sodium, more effervescent materials such as combinations of citric acid and sodium bicarbonate and/or sodium carbonate, lubricants to facilitate tablet retention such as magnesium stearate, etc. good.

Generally, the perborate portion is mixed with the polymeric fluorocarbon in the form of a compacted granulated mixture (granules).

Additionally, one composition contains an effective amount of perborate monohydrate that is present in the composition but not in the compacted granulation mixture, ie, is not bound to the compacted granulation mixture. In other words, the amount of perborate monohydrate is 1
Since it is added to the composition as a separate ingredient rather than as a part, it is not trapped or present in the granulation mixture. Typically, up to about 11% by weight of the total acid group perborate monohydrate is added to the pressure! It may be added as a separate element from the amount of perborate monohydrate present in the 11-part mixture. Although a small amount of separately added perborate monohydrate may not prove effective, an amount of from about 7 to about 11 percent by weight of the total acid group is preferred.

The anhydrous perborate salt is typically present in the compacted granulation mixture at about 2% to about 8%, preferably from about 3% to about 5% by weight of the total acid group.
exists in an amount of Perborate monohydrate is typically present in the compacted granulation mixture in an amount of about 2 to about 8 Ii, preferably about 3 to about 8 percent by weight of the total composition. The ratio of anhydrous perborate to perborate monohydrate is typically about 1.5:
It is within the range of 1 to about 1=15. The compacted mixture also contains a polymeric fluorocarbon having a factor of about [J, 4 to about [J, 7] of the compacted mixture. Suitably, the compressed mixture is present in an amount of from about 5 to about 10 parts by weight of total acid, preferably from about 6 to about 9 parts by weight.

Bleach activators typically contain from about 5 to about 15 weight percent of total acid, preferably from about 5 to about 10 momme, and most preferably from about 6 to about 8 weight percent.
It is present in an amount of Jk%. Preferably, the bleach activator is N
, N, 1 6 filtration with light N'-tetraacetylethylenediamine (TAED).

Those skilled in the art will appreciate that in any composition, the total percentage of the various components of the composition is ioo.

The invention is more fully illustrated by the following examples.

Unless otherwise specified, all amounts expressed as percentages are percentages by weight.

Example 1 This example describes formulation 1 of m grains of the bleach activator of the present invention.

In this example, sodium perborate monohydrate 538
grams, anhydrous sodium perborate 83 grams, N,
N, 1c, N'-tetraacetylethylenediamine (
TAED) 200 grams, and grade E 5 A
Two grams of polynato difluoroethylene powder (E, 1. DuPont) were dry mixed.

Mixing takes place for approximately 1-6 minutes, after which the mixture is pressed into a 5 Q SCU (Strorxg Cobb Uni
ts) into hard tablets with greater hardness. The granules were then passed through a vibratory granulator equipped with a 12 mesh size screen.

Example 2 296 grams of sodium perborate monohydrate, 182 grams of anhydrous sodium perborate were used in combination with polytetrafluoroethylene and TAED #1
Example 10 was repeated. The resulting granules had a hardness comparable to that of Example 1.

Example 5 A denture cleaning composition was prepared by blending the bleaching activator granules prepared in Example 1. The specific ingredients of the denture cleaning composition are shown in Table 1 below.

Table I Denture cleaning composition Sodium bicarbonate t7sP Granuleya 5 0.3420 Dye 0.0051
water o, o
os.

Technical Grade Ingredients Amount (grams)/-Tablet Sodium Carbonate (Soda Ash Density) 0.285
0 Citric Anhydride USP Fine Pl Granules α1
190 Anhydrous Sodium Sulfur 0
．． 1500 potassium monopersulfate
12210 Mint fragrance 600
0 Surfactant 0.0200 Excipient 0.0460 Polytetrafluoroethylene powder 0.002
8 Bleach activator granules (Example 1) 0. <
2i2''
The tablets were compressed into tablets using a tablet compressor with a tablet die. Each tablet weighs approximately 3.55 grams and is
It had a hardness of approximately 16 SOU with an oerlein blade. The tablets are 0.2 inches thick and tested to contain 115 ag of available oxygen per tablet in 120 ml of water at 45°C.
．． The longest disintegration time was 180 seconds.

The performance of this tablet was above average in the measurements fi, and tablets containing the bleaching activator granules of the present invention were determined to be desirable for use in denture cleaning compositions in tablet form.

Example 4 A denture cleaning composition of the present invention was prepared according to the formulation shown in Table 1. In this formulation, the bleach activator (TεD) was added to the composition without first incorporating it into the granules.

Table ■ Denture cleaning composition pre-granulated anhydrous sodium perborate 14188 Sodium perborate monohydrate 8Z06 Total pre-granulated
2!10.00 Final mixture sodium carbonate (soda ash density) 300.0
0 potassium monopersulfate sso, o.

Lathanol LAL powder 2L0
0 Pregranulation 23U, OO Anhydrous Sodium Tripolyphosphate 335.00 Sodium Bicarbonate USF Granules 5 56[,
OO dye
3.08 Citric Anhydride USP Fine Granules
125.00 ingredients
-i (r, 9/tablet) Sodium perborate monohydrate
265.00 flavor
30.00 Sodium benzoate 4
8.00 Sodium sulfate 160.
00T D 200.
00 Magnesium Stearate 1.0
0 Total Final Mixture 2,950.08 Table■
Pre-granulation was carried out in a similar manner to the preparation of bleach activator granules in Example 1, except that no bleach activator was added during the pre-granulation. That is, the ingredients of the pregranulation were mixed for about 1 to about 3 minutes and the mixture was compressed to form tablets having a hardness of 30 SCU. Thereafter, the tablets were crushed and the granules produced by the crushing were passed through a 20 mesh size sieve. Preparation of granulated perborate (pre-granulation)
H U.S. Pat. No. 4,405,486, the disclosure of which is incorporated herein by reference.

Although it is not critical to mix the components of the final mixture, magnesium stearate and polytetrafluoroethylene are mixed last.

Once all ingredients were added, the mixture was mixed for about 1 to about 3 minutes. There is no benefit to mixing for longer than 3 minutes since the hardness of the final tablet is reduced by increasing the mixing time. The mixture was then compressed to form tablets in a tablet compressor with a 27/32" diameter. Individual tablets weighed approximately 5.0 grams and weighed approximately 16 SC with an H6uberlein blade.
It had a hardness of U. The tablets were then cured in a heated air oven at about 90° C. for about 60 minutes. The tablets are approximately 0.2 inches thick and tested in water at 45°C (initial 3°C).
3115 ig/tablet of effective acid in 0 ml.

Keinaga's collapse took 180 seconds. When dissolved in about 120 milliliters of water, the composition exhibited a... of about 8.6.

Example 5 Tablets prepared from the denture cleaning composition of Example 4 were compared in cleaning ability with tablets prepared from the comparative composition shown in Table 1.

Table ■ Comparative denture cleaning composition ingredients 1 (slices/tablets) Sodium bicarbonate USP granules, jg 5 42
7.2 Citric Anhydride USP Fine Granules 316
．． 8 Sodium carbonate (soda ash density) 595A
Dye 2
72 water
10.00 Monopersulfuric acid compound
1.209.6 ingredients
Amount<W tablets) or powdered clay bar 31.0 Sodium benzoate 48.0 Magnesium stearate 6.72 Sodium perborate monohydrate 384.0 Mix the ingredients in Table m, and pour the resulting mixture into a die with a diameter of 27 mm. The tablets were compressed in a tablet compressor with a 32"
It had a hardness of 6 SCU.

The tablets were cured in a heated air oven at about 90C for about 60 minutes. The tablets are approximately 2 inches thick and have been tested in 120 milliliters of water at 45°C (initial temperature).
Available oxygen was 115 jli'/tablet, and the longest disintegration time was 180 seconds. When dissolved in about 120 ml of water,
The composition exhibited a - of about 8.6.

The compositions of the present invention in Table 1 were compared with the comparative compositions in Table 2 in an in vitro test for their ability to clean food and plaque stains from denture tiles. Denture tiles having coffee, tea, blueberry, and glaze stains on the StA matrix were prepared by dissolving approximately 3.0 gram tablets in approximately 120 milliliters of water at an initial temperature of approximately 45°C. It was immersed in the solution of the composition for 12 minutes.

Similarly, the initial temperature of the denture tile with an L profile was approximately 45°C.
The sample was immersed for 12 minutes in a solution of the composition of the invention of Table 3 prepared by dissolving about 50 gram tablets in about 120 milliliters of water.

The compositions of the present invention shown in Table 1 had improved cleaning ability compared to the comparative compositions shown in Table 3.

The present invention may be embodied in other forms or carried out in other ways without departing from its spirit or essential characteristics.

That is, the disclosure of the present invention is described in all respects 1) and is not intended to be limiting, and the scope of the present invention is considered to be indicated in the claims, and modifications that fall within the meaning and scope of equivalents are contemplated. , should be considered to be included in this.

Patent applicant Warner-Lampert Kompany et al.
given name

Claims (1)

Claims: 1) (i) a bleach activator selected from the group consisting of: (ii) anhydrous alkali metal perborate; and/or (iii) alkali metals, alkaline earth metals and mixtures thereof. and (iv) a polymeric fluorocarbon binder inert to bleach activators for use in washing, cleaning and/or bleaching compositions. Activator granules. 2) Bleach activator granules according to claim 1, wherein the alkali metal perborate anhydride is anhydrous sodium perborate. 3) Bleach activator granules according to claim 1, wherein the perborate monohydrate is sodium perborate monohydrate. 4) from about 5 to about 5 perborate anhydride based on the weight of the granules
Bleach activator granules according to claim 1 containing 0% by weight. 5) about 10 to about 50% by weight bleach activator, about 5 to about 50% by weight perborate anhydride, about 30 to about 60% by weight perborate monohydrate, based on the total weight of the granules. and from about 0.01 to about 1% by weight of a polymeric fluorocarbon. 6) Bleach activator granules according to claim 1, wherein the bleach activator is N,N,N',N'-tetraacetylethylenediamine. 7) The bleach activator granules of claim 1 having a particle size of about 10 to about 100 mesh. 8) Bleach activator granules according to claim 1, which have a pH ranging from about 10 to about 11.5 in an aqueous medium. 9) Bleach activator granules according to claim 1, wherein the binder is polytetrafluoroethylene. 10) (i) Based on the final composition, monopersulfate from about 20 to
(ii) a bleach activator; (iii) an anhydrous alkali metal perborate; and/or (iv) a metal perborate selected from the group consisting of alkali metals, alkaline earth metals, and mixtures thereof. borate 1
and (v) a polymeric fluorocarbon binder that is inert to the bleach activator, and at least a portion of the bleach activator and anhydrous perborate and/or perborate monohydrate and a polymer. An improved foamable cleaning composition in which a fluorocarbon binder is present in a compressed granule mixture. 11) The composition according to claim 10, wherein the phosphate is an alkali metal phosphate. 12) The composition according to claim 10, wherein the monopersulfate is sodium monopersulfate. 13) The composition according to claim 10, wherein the alkali metal perborate anhydride is anhydrous sodium perborate. 14) The composition according to claim 10, wherein the perborate monohydrate is sodium perborate monohydrate. 15) A composition according to claim 10, wherein the bleach activator is N,N,N',N'-tetraacetylethylenediamine. 16) A composition according to claim 10, wherein the polymeric fluorocarbon is polytetrafluoroethylene. 17) dry mixing an alkali metal perborate monohydrate and/or an anhydrous alkali or alkaline earth metal perborate and a polymeric fluorocarbon with a bleach activator for about 1 to about 3 minutes; , a method for preparing effervescent bleach activator granules comprising compressing the resulting mixture. 18) The method of claim 17, wherein the granules produced have a particle size of about 10 to about 100 mesh. 19) The method of claim 17, wherein the granules produced have a particle size of about 12 to about 30 mesh. 20) Bleaching where the alkali metal perborate monohydrate is sodium perborate monohydrate, the anhydrous perborate is anhydrous sodium perborate, and the polymeric fluorocarbon is polytetrafluoroethylene The activator is N, N,
18. The method of claim 17, wherein N',N'-tetraacetylethylenediamine. 21) (i) Based on the final composition, monopersulfate from about 20 to
from about 60% by weight; (ii) an effective amount of a bleach activator; (iii) an effective amount of an anhydrous alkali metal perborate; and/or (iv) an effective amount of alkali metals, alkaline earth metals, and mixtures thereof. a perborate monohydrate of a metal selected from the group consisting of; and (v) a polymeric fluorocarbon binder that is inert to an effective amount of a bleach activator and an anhydrous perborate. A foamable cleaning composition in which at least a portion of an acid salt and/or perborate monohydrate and a polymeric fluorocarbon binder are present in a compacted granular mixture. 22) A composition according to claim 21, wherein the bleach activator is N,N,N',N'-tetraacetylethylenediamine. 23) The bleach activator is about 5% to about 15% by weight of the total weight of the composition.
22. A composition according to claim 21, wherein the composition is present in an amount of . 24) A composition according to claim 21, wherein the granulation mixture contains anhydrous perborate and perborate monohydrate. 25) Anhydrous perborate and perborate monohydrate are approximately 1.5
25. The composition of claim 24, wherein the ratio ranges from :1 to about 1:1.5. 26) Anhydrous perborate is present in an amount ranging from about 2 to about 8% by weight of the total composition, and perborate monohydrate is present in an amount ranging from about 2 to about 8% by weight of the total composition. 25. A composition according to claim 24, wherein the composition is present in an amount. 27) (i) a monopersulfate from about 20 to about 60% by weight of the total composition; (ii) a bleach activator from about 5 to about 15% by weight of the total composition; (iii) an alkali metal perborate. anhydrous alkali metal perborate and perborate monohydrate selected from the group consisting of About 2% to about 8% by weight of the composition of anhydrous alkali metal perborate and about 2% to about 8% of the total composition of perborate monohydrate are present in the granulated mixture of polymeric fluorocarbons. 4 to about 0.7% by weight
present in the granulated mixture compressed with the granulated mixture, the ratio of anhydrous perborate to perborate monohydrate in the granulated mixture being in the range of about 1.5:1 to about 1:1.5. what is in;
and (iv) an effective amount of perborate monohydrate not present in the compressed granulation mixture, wherein the perborate monohydrate is an alkali metal perborate monohydrate. 1. A foaming cleaning composition, comprising: an alkaline earth metal perborate monohydrate; and a mixture thereof. 28) The composition of claim 21 or 27, wherein the perborate monohydrate not present in the compacted granulation mixture is present at about 7% to about 11% by weight of the total composition. 29) Perborate monohydrate is alkali metal perborate 1
The composition according to claim 21, which is a hydrate. 30) The composition according to claim 29, wherein the alkali metal of the anhydrous alkali metal monohydrate perborate is sodium. 31) Perborate monohydrate is alkali metal perborate 1
28. The composition according to claim 27, which is a hydrate. 32) The composition according to claim 31, wherein the alkali metal of the anhydrous alkali metal perborate and the alkali metal perborate monohydrate is sodium. 33) A composition according to claim 21 or 27, further comprising an effective amount of a detergent. 34) The composition according to claim 21 or 27, further comprising an effective amount of a chelating agent. 35) The composition according to claim 21 or 27, wherein the monopersulfate is potassium monopersulfate. 36) The monopersulfate is potassium monopersulfate and the perborate is anhydrous sodium perborate and sodium perborate monohydrate, and the perborate 1 is not present in the granulation mixture. 28. The composition of claim 27, wherein the hydrate is present in the composition in an amount from about 7 to about 11% by weight of the total composition. 37) The composition of claim 36 further comprising effective amounts of a detergent and a chelating agent.