MXPA00009525A - Stable, high available halogen 1,3,5-triazine-2,4,6-trione compositions having rapid dissolution rates - Google Patents

Abstract

Dry, stable, high available halogen sanitizing granular compositions with a rapid rate of dissolution comprising halogenated 1,3,5-triazine-2,4,6-triones and a dissolution accelerant that is an alkali metal salt of 1,3,5-triazine-2,4,6-trione are disclosed. The disclosed compositions may include inorganic and/or organic disintegration agents. Additionally, these compositions may contain other performance enhancing additives such as water clarifiers, algaestats/algaecides, surfactants, glidants, processing aids, and binders. These UV stable sanitizing compositions contain a high available halogen content, and are stable even when stored in high-humidity environments.

Description

COMPOSITIONS OF 1, 3,5-TRIAZIN-2,, 6-TRICETONE WITH HALOGEN HIGH AVAILABILITY, STABLE, THAT HAVE DISSOLUTION SPEEDS R REQUESTS The present invention relates generally to disinfectant compositions for controlling microbial growth in water recirculation systems, and more particularly to stable 1, 3, 5-triazine-2, 4,6-tricetone compositions with high halogen availability at a high speed rapid dissolution BACKGROUND OF THE INVENTION Halogen compounds, particularly those with chlorine and bromine, have long been used as disinfectants to kill bacteria, fungi, and algae in water recirculation systems. These halogen compounds, disinfectants are relatively low in cost and provide broad spectrum control at equally low concentrations (ppm).

Sodium hypochlorite, lithium hypochlorite, and calcium hypochlorite are among the most popular halogen-containing disinfectants, in part because they have high dissolution rates or are dispersed. REF. 123349 quickly in water. This feature is beneficial when it is necessary to provide high levels of halogen for water recirculation systems in a short period of time (often referred to as feed with drag, detachment of internal scale from the heating surfaces by change in the internal pressure of a serpentine, or superchlorination).

Of the disinfectant compounds with inorganic halogen, the calcium hypochlorite, which contains from 65% to 75% available halogen, is the dry granular material, more widely used because of its low cost and high halogen content. Sodium hypochlorite and lithium hypochlorite, compounds also capable of disinfecting, are less cost-effective and have less halogen availability in relation to calcium hypochlorite.

A significant inefficiency of all the above inorganic compounds is their susceptibility to degradation by ultraviolet (UV) rays when used in an outdoor water recirculation system. As is known in the art, UV rays reduce the levels of halogen in water, thus reducing the capacity of inorganic compounds to disinfect and purify.

To overcome this inefficiency, previously in the specialty inorganic compounds were used in combination with independent UV stabilizers, of which, the best known to overcome this inefficiency is 1, 3, 5-triazin-2,4,6-tricetone (cyanuric acid).

A more specific problem is associated with calcium hypochlorite. "The National Fire Protection Association" (NFPA) classifies calcium hypochlorite as a class 3 oxidant. The NFPA code defines a class 3 oxidant as "an oxidant that will cause a severe increase in the rate of burning of combustible materials. with which it is put in contact or that will undergo vigorous self-sustained decomposition due to contamination or exposure to heat ", NFPA 430: Code for the storage of Solid and Liquid Oxidants, 1995 edition, p.430-5.

An alternative for inorganic halogen disinfectant compounds is the class of 1, 3, 5-triazin-2,4,6-halogenated tricetones. The acid forms of 1, 3, 5-triazin- 2, 4, 6-tricetonás such as 1, 3, 5-trichloro-l, 3, 5-triazin- 2,4,6-tricetone (trichloroisocyanuric acid) and dichloro - ^^^ sÉÜ ^^ 1, 3, 5-triazina-2,4,6-tricetone (dichloroisocyanuric acid) have high availability of halogen, 90% and 70% respectively. The content of halogen of high availability and the intrinsic UV stabilizer (cyanuric acid), contained in these materials, provides an effective cost, widely used disinfectant compound, to treat external systems of water recirculation. NFPA classifies halogenated 1, 3, 5-triazine-2,4,6-tricetone as a Class 1 oxidant. NFPA defines Class 1 oxidants as "an oxidant whose primary risk is that it slightly increases the rate of combustion but does not causes spontaneous ignition when in contact with combustible materials, "NFPA 430: Code for the Storage of Liquid and Solid Oxidizers, 1995 Edition, p. 430-5.

However, halogenated 1, 3, 5-triazin-2,4,6-trichketones have slow dissolution rates as a result of low solubility. This makes the less desirable 1,3,5-triazine-2,4,6-trichetones halogenated when rapid release of the halogen is desired. In view of this limitation, compositions similar to trichloroisocyanuric acid have been compressed into tablets and used under conditions where a slow and constant release is desired. For example, feeding with continuous or semi-continuous erosion of these compositions has been effective in releasing a disinfecting amount of hypochlorous acid over a period of days as reported in US Pat. Nos. 5,648,314 to Lac Ocki et al., 5,514,287 to Jones. and collaborators, 5,510,108 from Chouraqui, and 5,498,415 from Jones.

Other organic alternatives for 1, 3, 5-triazin-2,4,6-trichketones for applications where rapid release of the halogen is desired are the anhydrous salts of the acids of the alkali metals (eg, sodium dichloroisocyanurate or potassium). The sodium and potassium dichloroisocyanurate salts are effective disinfectants, but they have reduced availability of halogen (62% and 58% respectively). In addition, these salts are classified by NFPA as Class 3 oxidants. Sodium dichloroisocyanurate can be hydrated, reducing the classification of NFPA oxidant to a Class 1 oxidant, but additional hydration of sodium dichloroisocyanurate reduces the available halogen content. making the disinfectant compound less effective in cost.

The following table compares the important characteristics of the disinfectant compounds with halogen previously described.

Oxidants are classified on a scale of 1 to 4 based on the codes of the "National Fire Protection Association" (NFPA). NFPA 430: Code for the Storage of Liquid and Solid Oxidants, 1995 edition.

Solubility in water at 20 ° C reported as g / 100 g (%) 3The Proper Management of Pool and Spa Water, Hydrotech Chemical Corporation, 1988 4Swimming Pool Disinfection with Chlorinated-s-Triazine Trione Products, Special Report 6862, Monsanto Company, May 1975.

Various attempts have been made to develop the disinfectant composition 1, 3, 5-triazin-2,4,6-tricetone with high availability of halogen, commercially feasible that dissolves rapidly. For example, Wojto icz describes rapid dissolution mixtures containing trichloroisocyanuric acid and alkali metal bicarbonates in US Patent No. 4,389,318. Wojtowicz also discloses rapid dissolution mixtures containing trichloroisocyanuric acid and alkaline earth metal salts of carbonate, hydroxide, and mixtures thereof in US Patent Nos. 4,472,187 and 4,498,921. In US Patent 4,599,411, Wojtowicz discloses a mixture of trichloroisocyanuric acid, cyanuric acid, and sodium bicarbonate. However, the Wojtowicz mixes were never commercialized.

However, there is a need for disinfectant compositions of stable halogenated 1, 3, 5-triazin-2, 4,6-tricetone, high dissolution speed with high available halogen content. There is also a need for halogen fast release disinfectant compositions that have a substantially longer lifetime in the presence of UV rays than inorganic halogen compositions. Additionally there is a need for disinfectant compositions having large amounts of halogen available in combination with other additives that provide benefits to the water recirculation systems. The present invention addresses all of these needs.

BRIEF DESCRIPTION OF THE INVENTION In one aspect briefly describing the invention, a disinfectant composition with halogen high availability, stable with a rapid dissolution rate comprising a halogenated 1, 3, 5-triazin-2,4,6-tricytone and an accelerator was provided. the solution which is an alkali metal salt of 1, 3, 5-triazin-2,4,6-tricetone.

In a further aspect of the present invention, the dissolution accelerator is replaced or supplemented with inorganic or organic disintegrating agents.

In another aspect of the invention the dry, stable, high availability halogen disinfectant composition further comprises chemicals that further improve water, including: water clarifiers, flocculants, coagulants, algicosets / algaecides, and / or fungicides.

In yet a further aspect of the invention, other ingredients such as colorants, surfactants, binder, etc. may be included.

An object of the present invention is to provide a rapidly dissolving disinfectant composition of a high availability of halogen, low solubility disinfectant,, with the formulation being stable during manufacturing and long term storage.

A further object of the present invention is to provide a rapidly dissolving, UV-stable disinfectant composition with a high available halogen content.

A further object of the present invention is to provide a method of applying the composition of the present invention to recirculating water.

Additional aspects and advantages of the present invention will be obvious from the following description.

BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a graph of the data presented in Table 10, and discloses halogen release, halogen stability, and clarity of water for one of the inventive compositions compared to calcium hypochlorite.

DESCRIPTION OF THE PREFERRED MODALITY For the purpose of providing a further understanding of the principles of the invention, reference is made to the preferred embodiments of the present invention, and specific language will be used to describe it. However, it will be understood that no attempt is made to limit the scope of the invention with this, as far as the invention pertains to such alterations and further modifications to the illustrated invention, and such additional applications of the principles of the invention as illustrated herein. they are contemplated, as they normally take place, for an expert in the field.

The present invention provides rapidly dissolving, disinfecting compositions comprising a halogenated 1,3,5-triazin-2,4,6-tricytane, and an alkali metal salt of 1,3,5-triazine-2, 4 , 6-tricetone. An organic or inorganic disintegrating agent can also be included to supplement or replace the alkali metal salt. Finally, other additives that provide additional advantages to water recirculation systems including water clarifiers, flocculants, coagulants, algichates / algaecides (and / or fungicides), dyes, surfactants, binders, etc. may be included.

The inventive compositions are surprisingly stable, also when they are contaminated by water. Accordingly, they are useful for providing disinfectant, clarifying, and algicidal / algicidal components for water recirculation systems similar to swimming pools, spas, hot tubs, bath tubs, reflective assemblies, industrial water systems, fountains, etc. The relative proportions of the various components, as well as potential substitutions, are therefore written below. Representative examples of the preparation and use of the compositions are also presented.

As indicated above, 1, 3, 5-trichloro-1,3,5-triazin-2,4,6-trichketone (trichloroisocyanuric acid) is the preferred disinfectant used in the present invention, but it can be replaced by another with highly available halogen (e.g., more than 65% halogen available), low solubility oxidants such as other halogenated 1, 3, 5-triazin-2,4,6-trichketones. In the preferred embodiments, the disinfectant has an available halogen content of at least 70% (more preferably more than 85%), and a solubility in water at 20 ° C of less than about 2% weight / volume).

The concentration of trichloroisocyanuric acid or its substitute in the compositions of the present invention is between about 40% to about 99% by weight. Preferably the trichloroisocyanuric acid is present in an amount between about 50% to about 90% by weight, and more preferably between about 60% to about 80% of the total weight of the composition. Accordingly, in the most preferred embodiment, the compositions contain between about 54% to about 72% available halogen.

In the preferred embodiment of the invention, a dissolution aid such as an alkali metal salt of 1,3,5-triazin-2,4,6-trichketones is used. In producing the salt, the alkali metal reacts with 1, 3, 5-triazin-2, 6-tricetone to form the mono-, di-, or tri-metal alkaline salts. Sodium or potassium are the preferred alkali metals that can be donated by sodium hydroxide, sodium carbonate, sodium bicarbonate, and the like or analogues thereof of potassium. Sodium hydroxide is the most preferred donor. In the most preferred embodiment, the disodium salt of 1, 3, 5-triazin-2,4,6-tricetone (sodium cyanurate) is used.

The dissolution aid is added to the composition between about 1% to about 60%. In the preferred embodiment of the invention, between about 5% and about 40% is added, with about 8% to about 20% being most preferred.

Highly alkaline components mixed with trichloroisocyanuric acid are well known in the art for decomposing trichloroisocyanuric acid in said mixture. It was surprising, however, to find that highly alkaline salts (eg, disodium cyanurate) did not react to decompose trichloroisocyanuric acid in either wet or dry environment. These environmental conditions may be present during the manufacture or storage of the product.

In an alternative embodiment of the invention, the disodium cyanurate can be supplemented or replaced by one or more disintegrating agents that differ in the composition of 1,3,5-triazin-2,4,6-tricetone. Various inorganic or organic disintegrating agents can be used alone or in combination to increase the dissolution rate of trichloroisocyanuric acid. Useful inorganic agents include montmorilinite (for example, smectite, hectorite, and bentonite), laponite, and other clays that sponge when exposed to water. Of these, natural or synthetic montmorilinite or laponite clays are most preferred. Amorphous silica could also be used, as a disintegrating agent and as a binder. These compounds can be applied between about 0.1% to about 20%, with between about 1% to 10% being preferred.

They can also be used, organic disintegrating agents. Organic disintegrating agents include methyl cellulose, carboxymethyl cellulose, polyacrylamide and / or high molecular weight polyacrylate polymers, polyvinyl pyrrolidone or the crosslinked forms thereof. These compounds can be applied to the composition between about 0.1% to about 20%, with between about 1.0% to 10% being preferred.

Water clarifying agents known in the art (also known as coagulants and flocculants) can also be added. Preferred water clarifying agents are aluminum-containing complexes selected from the group of aluminum sulfate, aluminum chlorohydrate, sodium aluminum sulfate complex, aluminum potassium sulfate complex and the like. Hydrated aluminum sulfate is preferred. More preferred is aluminum sulfate having from about 2 to about 20 equivalents of water per mole of aluminum. In alternative embodiments, the complex containing aluminum sulfate is a hydrated aluminum potassium sulfate complex, the hydrated sodium aluminum sulfate complex, or the like. The concentration of the clarifying agent in water may contain between about 1% to about 40%. Preferably the water clarifying agent is present between about 2% to about 30. In the most preferred embodiment, the water clarifying agent is present between about 4% to about 18%.

The fast dissolving rate disinfectant composition also preferably includes an algicide / liguicide (and / or fungicide) additives such as the boron-containing compounds are selected from the group consisting of: boric acid, boric oxide (anhydrous boric acid), compounds that have the formula MnBxOy.ZH20 (in which M is any alkali metal or alkaline earth cation, including, but not limited to, sodium, potassium, calcium and magnesium; n is equal to, 2 or 3; x is any integer from 2 to 10, Y equals 3 X / 2 + 1, and Z equals 0 to 18). The compounds MnBxOy.ZH20, which contain boron include: sodium tetraborate, disodium octaborate, sodium pentaborate, sodium metaborate, dipotassium tetraborate, potassium pentaborate and hydrates thereof. The rapid dissolution rate disinfectant composition contains the compounds with boron in amounts between about 1% to about 40, more preferably about 2% to about 30%. In the most preferred embodiment, sodium tetraborate pentahydrate is present between about 4% to about 18%.

The disinfectant compositions of the present invention are preferably granular solid products of any size or shape of approximately 200 microns in diameter. The disinfectant compositions of granulated trichloroisocyanuric acid are preferred over disinfectant compositions of trichloroisocyanuric acid sprayed because of the inherent inhalation risk of the powders (respirable powders are particles or agglomerates of particles less than about 10 microns in diameter). The preferred embodiment reduces this risk by processing the pulverized components into larger non-respirable granules. A powder form of the disinfectant composition of the invention can be processed and can dissolve to a faster rate than the granules due to the greater surface area of the powders in proportion to the volume; however, the increase in handling risk for application is not desirable in the present invention. The granules of the disinfectant compositions of the present invention are prepared by dry particle size amplification methods, preferably co-compaction or granulation.

Additional components such as binders, tableting aids, molding releasing agents, corrosion inhibitors, scale inhibitors, surfactants, binders, or colorants may be incorporated into compositions of the present invention or to the final granulated product. The selection of such components depends on the skill of those skilled in the art.

In preparing the disinfectant composition of the present invention, the powder form of all components are mixed using the appropriate equipment selected by those skilled in solid material processes. The mixed material is then processed into granules using appropriate equipment known to those skilled in dry particle size enlargement.

The compositions of the present invention are preferably used to treat water recirculation systems such as swimming pools, spas, hot tubs, bath tubs, reflective assemblies, industrial water systems, fountains, etc. The present invention disinfects, clarifies, and reduces algae in water systems by contacting an effective amount for disinfecting the disinfectant composition of the present invention with the water system through an appropriate application method. Suitable amounts and methods of application can be determined by experts in the field without undue experimentation. Such methods of application can be manual or automatic.

Reference will be made to specific examples. It is understood that the examples are provided to more fully describe the preferred embodiments, and do not attempt to limit the scope of the invention.

Example 1 The procedure for Example 1 is generally as follows. This process is used to formulate components in halogen-containing materials such as trichloroisocyanuric acid on a small scale. The test helps identify materials that increase or decrease the stability of a formulation that contains a stable halogen material. Specifically, the addition of various components to the halogen-containing material can result in changes in the degassing profile of the halogen in the formulation. A titration with sodium thiosulfate is used to determine the degassing profile of the formulation. The thiosulfate titre is proportional to the amount of gaseous oxidant (chlorine, chloramine, etc.) released from the sample of the formulation during the test. Larger titers indicate greater gasification - a result indicating less stability in the formulation. Reciprocally, lower titles are indicators of greater stability in the formulation. The results of the test are used to guide decisions in the addition of components to the formulation.

Mixed powder samples were prepared for each composition of the formula. A two gram sample of each test formulation was placed in a 0.75 inch diameter punch filling machine and compressed with 400 Lbs of force for 15 minutes.

After a fifteen-minute cycle, the small pellet produced was transferred to an eight-ounce dry sample container. In Example 1, a small beaker containing 5 ml of 15% potassium iodide (Kl) was placed on the side of the tablet in the container, and the container was sealed with steam. The container (with the sample and beaker with Kl) was carefully placed in an oven at approximately 50 ° C for 24 hours. After the sample kit was removed from the oven and cooled, a 1 ml aliquot of each sample was placed in 50 ml of deionized water and titrated with 0.100 N sodium thiosulfate. The volume of thiosulfate reagent used for titration was recorded. the halogen available in the Kl solution.

The results of Example 1 (Table 1) demonstrate that high levels of aluminum sulfate, used as a water clarifier, and boric acid used as a lubricant in the drying process, do not significantly affect the degassing profile of trichloroisocyanuric acid. This is further documented in U.S. Patent No. 5,674,429. The results also show that sodium tetraborate pentahydrate, used as an alguistático, sodium bicarbonate and sodium carbonate, both used as dissolution aids, significantly increase gasification.

Table 1. Degassing of several trichloroisocyanuric acid formulas in compressed powder.

Formulation Title (ml) 100% trichloroisocyanuric acid 2.65 74. 5% trichloroisocyanuric acid and 25.5% aluminum sulfate 3.05 74. 5% trichloroisocyanuric acid and 25.5% boric acid 1.10 74. 5% trichloroisocyanuric acid and 25.5% sodium tetraborate pentahydrate 12.75 74. 5% trichloroisocyanuric acid and 25.5% sodium bicarbonate 15.05 74. 5% trichloroisocyanuric acid and 25.5% sodium carbonate 7.5 Example 2 Example 2 used the procedure described above for Example 1, except that the Kl beaker contained 10 ml of 30% Kl. For Example 2, each formulation contained fixed amounts of aluminum sulfate (8%) and boric acid (1%). The levels of these two components were set as a result of the data obtained in Example 1.

The results of Example 2 (Table 2) show that sodium tetraborate pentahydrate had a reduced tendency to cause degassing in the presence of aluminum sulfate as established in US Patent No. 5,674,429. The results also show that both sodium bicarbonate and sodium carbonate substantially increase the degassing of the trichloroisocyanuric acid formulations. Because of this relatively high degassing, an instability signal, no additional processes are attempted with these two additives.

Table 2. Degassing of several trichloroisocyanuric acid formulas in compressed powder, containing 8% aluminum sulfate and 1% boric acid.

Formulation Title (ml) 91. 5% trichloroisocyanuric acid 1.05 74. 5 trichloroisocyanuric acid and 16.5% sodium tetraborate pentahydrate 3.10 74. 5% trichloroisocyanuric acid and 16.5% sodium bicarbonate 8.95 74. 5% trichloroisocyanuric acid and 16.5% sodium carbonate 8.95 Example 3 Example 3 was developed to approach the co-compaction process. Co-compaction is a typical method used for dry particle size enlargement. The compositions of the formulas produced in this example were tested for their stability and in some cases for their solubility. The components used included a dissolving aid: disodium cyanurate, and a disintegrating agent: microcrystalline cellulose, Lattice® NT (FMC).

Again, the mixed powder samples were prepared for each formulation. A 20 g sample of each test formulation was placed in a 2.0 inch diameter punch filling equipment and compressed to 22 tons of force for 60 minutes using the Carver compressor.

The compressed tablet was reduced to granules using a spatula and mortar and grinder equipment. The appropriately sized granules were collected using a standard mesh stirrer.

Approximately one gram of sample of each composition of granular formula was placed in an 8-ounce sample container. A beaker with 5 ml of 30% Kl solution was placed in each sample container. The containers were steam sealed and carefully placed in an oven at approximately 50 ° C for 24 hours. After the sample kit was removed from the oven and cooled, a 1 ml aliquot of each sample was placed in 50 ml of deionized water and titrated with 0.100N sodium thiosulfate. The volume of thiosulfate reagent used for titration was recorded. the halogen available in the Kl solution. The results are shown in Table 3.

The results of Example 3 (Table 3) show the formulations containing constant levels of trichloroisocyanuric acid, aluminum sulfate, and boric acid with varying levels of disodium cyanurate, used as a dissolution aid, sodium tetraborate pentahydrate, used as an algae / algaecide, do not significantly affect the degassing profile of the compositions of the trichloroisocyanuric acid formula. Microcrystalline cellulose, used as a disintegrating agent, moderately impacts the degassing of trichloroisocyanuric acid.

Table 3. Degassing of several granular trichloroisocyanuric acid formulas containing 8% aluminum sulfate and 1% boric acid.

Formulation Title (ml) 91% trichloroisocyanuric acid 0.35 82. 75% trichloroisocyanuric acid and 8.25% disodium cyanurate 0.40 74. 5% trichloroisocyanuric acid and 16.5% sodium tetraborate pentahydrate 0.30 74. 5% trichloroisocyanuric acid and 16.5% disodium cyanurate 1.40 74. 5% trichloroisocyanuric acid and 16.5% Lattice® NT 4.40 74. 5% trichloroisocyanuric acid and 8.25% disodium cyanurate, and 8.25% sodium tetraborate pentahydrate 0.60 Some of the relatively stable formulas reported in Table 3 were also tested for solubility using the following method. A sample of one gram of the formulation to be tested was placed in 200 ml of a balanced pool water solution. The balanced pool water contained approximately 200 ppm of calcium hardness and 125 ppm of total alkalinity (pH = 7.5). A table stirring device that did not have a physical agitator apparatus (e.g., stir bar or paddle) gently agitated the samples for 15 minutes. This gentle agitation allowed a simulation of more real dissolution with the material that was dissolved by the movement of the water, preferably to the physical crushing caused by the agitators and paddles.

After a dissolution period of 15 minutes, the sample solution was filtered to remove any remaining insoluble granules. An aliquot of 1 ml of the solution of the filtered sample was placed in 25 ml of deionized water. The halogen content available in the aliquot of the sample solution was titrated with 0.010 N sodium thiosulfate. All measurements were made in milliliters (ml) of titrant. A great title is an indicator of a highly soluble formula. A titre close to 9.6 ml of 0.010 N sodium thiosulfate would indicate that all available halogen was completely dissolved in a 72.2% trichloroisocyanuric acid formulation with approximately 65% available halogen). Calcium hypochlorite with 65% available halogen and a fast dissolution rate was used as a control.

The solubility data of Example 3 (Table 4) show that the 8.25% disodium cyanurate formulation dissolves twice as fast as 100% trichloroisocyanuric acid. Additionally, the dissolution rate of the formulation containing 16.5% disodium cyanurate is four times faster than the dissolution rate of 100% trichloroisocyanuric acid. The dissolution rate of the formulation containing 16.5% microcrystalline cellulose is twice the dissolution rate of trichloroisocyanuric acid. The formulation containing 8.25% disodium cyanurate and 8.25% sodium tetraborate pentahydrate exhibited an improved dissolution rate in relation to 100% trichloroisocyanuric acid.

Table 4. Solubility of several granular trichloroisocyanuric acid formulas containing 8% aluminum sulfate and 1% boric acid compared to 100% trichloroisocyanuric acid and calcium hypochlorite.

Formulation Title (ml) Calcium hypochlorite (65% available chlorine) 9.6 100% trichloroisocyanuric acid 0.8 82. 75% trichloroisocyanuric acid and 8.25% disodium cyanurate 1.70 74. 5% trichloroisocyanuric acid and 16.5% disodium cyanurate 3.20 74. 5% trichloroisocyanuric acid and 16.5% Lattice® NT 1.70 74. 5% trichloroisocyanuric acid and 8.25% disodium cyanurate, and 8.25% sodium tetraborate pentahydrate 2.00 Example 4 The procedure of Examples 4-6 is as follows. Approximately 4 to 6 pounds of formulations of mixed powder samples were prepared. The samples were processed into granules using a pilot scale roller compactor, mill, and mesh stirrer.

For Example 4, a formulation containing 74.5% trichloroisocyanuric acid, 8% aluminum sulfate, 9% sodium tetraborate pentahydrate, 5% disodium cyanurate, and 0.5% Cab-O-Sil® (CABOT), it was formulated. Several disintegration agents and a surfactant were added to this formulation.

In Example 4, stability tests were performed by adding one gram of appropriately calibrated granules to an 8-ounce jar. A beaker containing 5 ml of a 30% solution of Kl was placed in each sample container. Additionally, 100 μl of distilled water was added to contaminate the trichloroisocyanuric acid formulation. Moisture contamination is used to "fatigue" the system in relation to stability. Each test jar was steam sealed and the sample containers were carefully placed in an oven at approximately 50 ° C for 24 hours. After the equipment with the sample was removed from the oven and cooled, a 1 ml aliquot of each sample was placed in 50 ml of deionized water and titrated with 0.100 N. sodium thiosulfate.

The stability data of Example 4 (Table 5) show that relatively stable formulas containing a dissolution aid, disintegration agents, and / or a surfactant can be co-compacted into granules. The organic dissolving aid polyvinyl pyrrolidone (Sigma) was the least stable in this group of samples. GelWhite L inorganic clays (Southern Clay Products) and Van-Gel® O (Vanderbilt) were relatively stable. The surfactant Hostapur SAS 93G (Clariant) was also relatively stable in the formulation.

Table 5. Degassing of several granular trichloroisocyanuric acid formulas containing 8% aluminum sulfate, 9% sodium tetraborate pentahydrate, 5% disodium cyanurate and 0.5% Cab-O-Sil® Formulation Title (ml) 74. 5% trichloroisocyanuric acid and 3% GelWhite L 2.2 74. 5% trichloroisocyanuric acid and 3% Van-Gel® O 2.8 74. 5% trichloroisocyanuric acid and 3% polyvinylpyrrolidone 4.4 74. 5% trichloroisocyanuric acid and 3% Hostapur SAS 93G 2.10 Solubility tests were carried out in Example 4 in the same manner as in Example 3. In Example 4, the formulation with Van-Gel® O had the highest rate of dissolution in relation to all the other additives tested. Additionally, Gel-White L, polyvinylpyrrolidone, and HostaPur SAS 93G significantly improved the rate of dissolution. The results were recorded in Table 6.

Table 6. Solubility of several granular trichloroisocyanuric acid formulas containing 8% aluminum sulfate, 9% sodium tetraborate pentahydrate, 5% disodium cyanurate and 0.5% Cab-O-Sil® Formulation Title (ml) 74. 5% trichloroisocyanuric acid and 3% GelWhite L 3.3 74. 5% trichloroisocyanuric acid and 3% Van-Gel® 0 4.90 74. 5% trichloroisocyanuric acid and 3% polyvinylpyrrolidone 3.25 74. 5% trichloroisocyanuric acid and 3% HostaPur SAS 93G 3.05 Example 5 A formulation containing 72.5% trichloroisocyanuric acid, 8% aluminum sulfate, and 8% sodium tetraborate pentahydrate was prepared. Again, several disintegration agents were added to the formulation. Additionally, a binder was added. The formulation was processed as described below.

The stability results of Example 5 (Table 7) show that the formulation containing 11.5% of disodium cyanurate had greater stability in relation to all the other formulations evaluated. Two formulations, one containing 4% of Hectabrite AW (American Coloid Co.), 3.0% of Vee-Gum® T (Vanderbilt) and 4.5% of disodium cyanurate and the other containing 3.0% of Vee-Gum® T and 8.5 Disodium cyanurate% were relatively stable in Example 5. Finally, two other formulations, one containing 1.75% Hectabrite AW, 3.0% Vee-Gum® T, 5% Van-Gel® O, and 1.75% Cab -O-Sil® and the other that contained 4.0% Hectabrite AW, 2.5% Vee-Gum® T, and 5.0% Cab-O-Sil® were not stable, but could potentially be used, depending on the application.

Table 7. Degassing for a formula containing 72.5% trichloroisocyanuric acid, 8% aluminum sulfate, 8% sodium tetraborate pentahydrate.

Formulation Title (ml) 72.5% trichloroisocyanuric acid and 1.75% Hectabrite AW, 3.0% Vee-Gum T, 5% Van-Gel-O, and 1.75% Cab-O-Sil® 3.85 72. 5% trichloroisocyanuric acid and 4% Hectabrite AW, 2.5% Vee-Gum T, and 5% Cab-O-Sil® 3.50 72. 5% trichloroisocyanuric acid and 4% Hectabrite AW, 3% Vee-Gum T, and 4.5% disodium cyanurate 1.50 72. 5% trichloroisocyanuric acid and 3% Vee-Gum T, and 8.5% disodium cyanurate 1.60 74. 5% trichloroisocyanuric acid and 11.5% disodium cyanurate 1.00 The solubility data of Example 5 (Table 8) show that the solubility rates for the formulations of Example 5 as well as a mixture of trichloroisocyanuric acid and sodium carbonate. The results indicate that the more stable formulation of Table 7 (11.5% disodium cyanurate) had an increase in dissolution rate in relation to 100% trichloroisocyanuric acid. This rate of dissolution is slightly better than the rate of dissolution of the relatively unstable mixture of trichloroisocyanuric acid and sodium carbonate. Overall, the formulation containing 1.75% of Hectabrite AW, 3.0% of Vee-Gum® T, 5% of Van-Gel® O, and 1.75% of Cab-O-Sil® had higher dissolution rate. Another relatively stable formulation such as: 4.0% Hectabrite AW, 2.5% Vee-Gum® T, and 5.0% Cab-O-Sil®; 4.0% of Hectabrite AW, 3.0% of Vee-Gum® T, and 4.5% of disodium cyanurate and 3.0% of Vee-Gum® T and 8.5% of disodium cyanurate had good solubility rates as indicated in Table 8.

Table 8. Solubility for a formula containing 72.5% trichloroisocyanuric acid (65% available chlorine), 8% aluminum sulfate, 8% sodium tetraborate pentahydrate.

Formulation Title (ml) 72. 5% trichloroisocyanuric acid and 1.75% Hectabrite AW, 3.0% Vee-Gum® T, 5% Van-Gel® 0, and 1.75% Cab-O-Sil® 6.28 72. 5% trichloroisocyanuric acid and 4.0% Hectabrite AW, 2.5% Vee-Gum® T, and 5.0% Cab-O-Sil® 5.08 72. 5% trichloroisocyanuric acid and 4% Hectabrite AW, 3.0% Vee-Gum® T, and 4.5% Disodium cyanurate 4.22 72. 5% trichloroisocyanuric acid and 3.0% Vee-Gum® T, and 8.5% disodium cyanurate 4.67 Formulation Title (ml) 72.5% trichloroisocyanuric acid and 11.5% disodium cyanurate 4.88 75% trichloroisocyanuric acid and 25% sodium carbonate 10 (Granular Mixture) 4.45 100% trichloroisocyanuric acid 0.8 Example 6 A formulation containing trichloroisocyanuric acid and disodium cyanurate was prepared. The formulation was processed as described above.

The data of Example 6 (Table 9) show that a formulation containing 60.0% of disodium cyanurate had reasonable stability in relation to the control of 100% trichloroisocyanuric acid. The solubility data for the formulation with 60.0% disodium cyanurate was 5.18 ml, markedly better than control. Theoretically, a title ^^ ^^ ^^^^^^ s approximately 5.4 ml of 0.010 N sodium thiosulfate indicate it complete solubilization of trichloroisocyanuric acid in the formulation with 60% disodium cyanurate.

Based on this theoretical calculation, the experimental data showed almost complete solubilization of the available chlorine in the experimental formulation.

Table 9. Solubility and Stability of Formulations with trichloroisocyanuric acid and disodium cyanurate.

Formulation Solubility Degassing title titer (ml) (ml) 100% trichloroisocyanuric acid 1.9 2.00 40. 0% trichloroisocyanuric acid and 60% disodium cyanurate 5.18 3.40 Example 7 Example 7 shows how the halogen disinfectant composition of example 5 containing 11.5% disodium cyanurate is compared to calcium hypochlorite in one application. This was accomplished by exposing beakers 2, 4 liter 3500 ml of water synthetic pool containing approximately 200 ppm calcium hardness and 125 ppm total alkalinity (pH = 7.5) to environmental UV rays by placing The signs on the outside on a sunny day. An equivocal amount of 10 ppm available halogen was added to each solution. The samples were periodically examined for chlorine and turbidity (NTU). The results were reported in Table 10. Additionally, Figure 1 graphically illustrates the reported data.

Table 10. Formulations with calcium hypochlorite compared to 1, 3, 5- trichloro-1, 3, 5-triazin-2, 4, 6-triketone, 1, 3, 5-triazin-2, 4, 6-triketone sodium, aluminum sulfate, and borax (Example 5); Test for halogen release, Halogen Stability, and water clarity.

Total Cl time: Total Cl: NTU: NTU: Composition Composite Hypochlorite- Hipo- ues- of the Calcium ion of the chloro- treo pio 5 Example to (Hr: 5 calcium min 0:00 0.02 0.02 0.23 0.29 0:05 4.1 0:10 5.1 6.8 Total Cl Time: Total Cl: NTU: NTU: Composition Composite Hypochlorite- Hipo-mues- from the calcium chloride formation example 5 Example to (Hr: 5 calcium min) 0:15 9.4 7.2 0.36 1.08 0:20 9.1 6.8 0:25 8.5 6.0 0:30 .1 5.1 0.19 1.02 0:40 .1 5.0 0.25 1.43 0:50 6.5 3.3 1:00 6.3 3.5 0.17 1.35 1:15 6.1 2.2 1:30 6.1 2.6 0.19 1.32 The results in Table 10 and Figure 1 illustrate that the halogen disinfectant composition of Example 5 has superior halogen release, superior UV degradation resistance, reduced turbidity relative to calcium hypochlorite .

While the invention has been illustrated and described in detail in the foregoing description, it is considered as illustrative and not restrictive of its character, it being understood that only the preferred embodiments have been disclosed and described, and that it is desired to protect all changes and modifications that are in the spirit of the invention.

It is noted that in relation to this date the best method known by the applicant to carry out the aforementioned invention is that which is clear from the present description of the invention.

Having described the invention as above, it is claimed as property in the following:

Claims (27)

1. A disinfectant composition, which is characterized in that it comprises: (a) between about 40% and about 99% of a 1, 3, 5-triazin-2, 6-halogenated tricetone; Y (b) between about 1% and about 60% of an alkali metal salt of 1,3,5-triazin-2,4,6-tricetone.

2. The disinfectant composition of claim 1 which is characterized in that said product comprises between about 60% and about 97% of 1,3,5-triazine-2,4,6-trichketone, and between about 3% to about 40% of a alkali metal salt of 1,3,5-triazin-2,4,6-tricetone.

3. The disinfectant composition of claim 1 which is characterized in that said 1,3,5-triazin-2,4,6-tricytone is 1, 3, 5-trichloro-1,3,5-triazine-2, 4,6- tricetone.

4. The disinfectant composition of claim 1 which is characterized in that said alkali metal salt of 1, 3, 5-triazin-2,4,6-tricetone is a sodium or potassium salt of 1, 3, 5-triazin-2, , 6-tricetone.

5. The disinfectant composition of claim 4 which is characterized in that said alkali metal salt of 1, 3, 5-triazin-2,4,6-tricetone is disodium cyanurate or dipotassium cyanurate.

6. The disinfectant composition of claim 1 which is characterized in that said composition additionally includes a second disintegrating agent, wherein said disintegrating agent differs in composition from 1,3,5-triazin-2,4,6-tricetone.

7. The disinfectant composition of claim 6 which is characterized in that said second disintegrating agent is present in an amount of between about 0.1% to about 20%.

8. The disinfectant composition of claim 6 which is characterized in that said second disintegrating agent is present in an amount of between about 1.0 to about 10%.

9. The disinfectant composition of claim 6 which is characterized in that said second disintegrating agent comprises an inorganic disintegrating agent selected from the group consisting of spongeable clays with natural water, clays spongeable with synthetic water, and amorphous silica.

10. The disinfectant composition of claim 6 which is characterized in that said second disintegrating agent comprises an organic disintegrating agent selected from the group consisting of cellulose compounds, high molecular weight polymers, and the crosslinked forms of said polymers.

11. The disinfectant composition of claim 1, and which are characterized in that they additionally include between about 1% to about 40% of an algogistic / algicidal and / or fungicidal compound.

12. The disinfectant composition of claim 11 which is characterized in that said algogistic / algicidal and / or fungicidal compound is present in an amount of between about 4% to about 18%.

13. The disinfectant composition of claim 12 which is characterized in that said algaetic / algicide and / or fungicide is a compound that liberates boron.

14. The disinfectant composition of claim 13 which is characterized in that said boron releasing compound is selected from boric acid, boric oxide (anhydrous boric acid), compounds having the formula MnB? O and ZH20 (wherein M is ammonium or any metal alkaline or alkaline-earth cation, which includes, but is not limited to, sodium potassium, calcium and magnesium, n is equal to, 2 or 3, x is any integer from 2 to 10, and is equal to 3X / 2 + 1; and Z equals 0 to 18).

15. The disinfectant composition of claim 14, which is characterized in that the boron releasing compound is sodium tetraborate pentahydrate.

16. The disinfectant composition of claim 1, which is characterized in that it includes between about 1% to about 40% of a water clarifier, coagulant or flocculant.

17. The disinfectant composition of claim 16 which is characterized in that said clarifier, coagulant or water flocculant is present in an amount of between about 4% to about 18%.

18. The disinfectant composition of claim 16 which is characterized in that said clarifier, coagulant or water flocculant is a complex that liberates aluminum.

19. The disinfectant composition of claim 16 which is characterized in that said aluminum releasing complex comprises an aluminum sulfate.

20. The disinfectant composition of claim 1, and further characterized in that it includes a surfactant.

21. The disinfectant composition of claim 1, and further characterized in that it includes a binder.

22. The disinfectant composition of claim 1, and further characterized in that it includes a process aid.

23. The disinfectant composition of claim 1, and further characterized in that it includes a binder.

24. A disinfectant composition, which is characterized in that it comprises: (a) between about 40% and up to about 99% of a halogenated 1, 3, 5-triazin-2,4,6-tricetone; Y (b) between approximately 0.1% and up to approximately 20% of a dissolution agent which differs in composition from the alkali metal salts of 1, 3, 5-triazin-2,4,6-tricetone.

25. The disinfectant composition of claim 24 which is characterized in that said dissolving agent comprises an inorganic disintegrating agent selected from the group consisting of spongeable clays with natural water, clays spongeable with synthetic water, and amorphous silica.

26. The disinfectant composition of the claim Which is characterized in that said dissolving agent comprises an organic disintegrating agent selected from the group consisting of cellulose compounds, high molecular weight polymers, and the crosslinked forms of said polymers.

27. A method of disinfecting water, said method being characterized in that it comprises adding to the water a disinfectably effective amount of a composition comprising: (a) between about 40% and about 99% of a halogenated 1, 3, 5-triazin-2,4,6-tricetone; Y (b) between about 1% and about 60% of an alkali metal salt of 1,3,5-triazin-2,4,6-tricetone.