Source: http://www.google.com/patents/US7465412?dq=7,346,545
Timestamp: 2017-05-24 15:00:46
Document Index: 377113643

Matched Legal Cases: ['art 173', '§173', '§173', '§173', '§173', '§173']

Patent US7465412 - Calcium hypochlorite composition - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inPatentsCalcium hypochlorite compositions that are classified as a Packing Group III Division 5.1 oxidizer material or as a non-Division 5.1 oxidizer material are described. In one embodiment, the compositions comprise an admixture of particulate calcium hypochlorite and particulate metaboric acid. The calcium...http://www.google.com/patents/US7465412?utm_source=gb-gplus-sharePatent US7465412 - Calcium hypochlorite compositionAdvanced Patent SearchTry the new Google Patents, with machine-classified Google Scholar results, and Japanese and South Korean patents.Publication numberUS7465412 B2Publication typeGrantApplication numberUS 11/065,231Publication dateDec 16, 2008Filing dateFeb 24, 2005Priority dateOct 28, 2004Fee statusLapsedAlso published asUS20060091356Publication number065231, 11065231, US 7465412 B2, US 7465412B2, US-B2-7465412, US7465412 B2, US7465412B2InventorsStanley R. Pickens, Fred Abraham, Donald W. DuBoisOriginal AssigneePpg Industries Ohio, Inc.Export CitationBiBTeX, EndNote, RefManPatent Citations (31), Referenced by (10), Classifications (8), Legal Events (14) External Links: USPTO, USPTO Assignment, EspacenetCalcium hypochlorite composition
US 7465412 B2Abstract
Calcium hypochlorite compositions that are classified as a Packing Group III Division 5.1 oxidizer material or as a non-Division 5.1 oxidizer material are described. In one embodiment, the compositions comprise an admixture of particulate calcium hypochlorite and particulate metaboric acid. The calcium hypochlorite is present in the composition in an amount and is of a concentration such that the composition would be classified as a Packing Group II Division 5.1 oxidizer in the absence of said particulate metaboric acid. Other embodiments described are solid shaped articles, e.g., tablets, comprising the described calcium hypochlorite-metaboric acid composition.
This application claims the benefit of U.S. Provisional Application Ser. No. 60/622,736 filed Oct. 28, 2004, which is herein incorporated by reference in its entirety.
The sanitization of a standing or recirculating aqueous medium typically involves introducing a hypohalite, e.g., a hypochlorite, anion donor material, such as a halogen or halogen-containing material, e.g., calcium hypochlorite, into the aqueous medium so as to establish a desired level, e.g., a sanitizing amount, of free available halogen, e.g., free available chlorine (FAC), within the aqueous medium. The presence of free available chlorine within the aqueous medium, e.g., a swimming pool, serves to eradicate or control deleterious amounts of pathogenic bacteria, algae, etc that are present in the aqueous medium. As an oxidizer, hypochlorous acid can also remove nutrients from the water, thus providing indirect protection against microbial infestation. Sanitation of water contacted by humans and animals is required because exposure to unsanitized or inadequately sanitized water that contains deleterious amounts of pathogenic bacteria, viruses, protozoa, etc can lead to the development of infection or disease.
In the case of a standing or recirculating body of water, e.g., swimming pools, periodic batch additions of higher levels of hypochlorite anion can be made to the body of water in addition to the relatively steady and lower level additions described previously. Such batch additions of higher levels of hypochlorite anion are commonly referred to as a “shock treatment” or as a “super chlorination” and are made on a periodic basis, e.g., once a week or once a month. Typically, the purpose of a shock treatment is to briefly increase the FAC of the body of water, e.g., by 5 to 20 ppm, to consume accumulated organic material, destroy chloramines and/or control algae blooms. A shock treatment is administered by, for example, preparing a concentrated aqueous solution of calcium hypochlorite from granulated calcium hypochlorite, and then adding this solution to the body of water, or distributing, e.g., broadcasting, granulated calcium hypochlorite directly over the surface of the body of water.
In accordance with Title 49, Code of Federal Regulations, part 173, section 127, paragraph (a), subparagraph (1), [49 CFR §173.127(a)(1)], calcium hypochlorite is categorized as a Division 5.1 oxidizer. It is classified as a Packing Group II oxidizer material [49 CFR §173.127(b)(ii)]. The transport of a material categorized as a Division 5.1 oxidizer requires the use of special precautions, which can include the use of special containers. The storage of NFPA (National Fire Protection Association) class 3 oxidizers (which UN Group II oxidizers will commonly be) can require separate free standing storage facilities and/or special sprinkler systems. Such special provisions for storage and handling can result in increased costs for these activities.
In accordance with the present invention there are provided, calcium hypochlorite compositions comprising an admixture of particulate calcium hypochlorite and particulate metaboric acid, which compositions are classified as a Packing Group III Division 5.1 oxidizer material or as a non-Division 5.1 oxidizer. The calcium hypochlorite used to prepare the foregoing compositions is present in an amount and is of a concentration such that said calcium hypochlorite compositions would be classified as a Packing Group II Division 5.1 oxidizer in the absence of an effective flame inhibitor, such as the herein described metaboric acid. In one embodiment, the calcium hypochlorite has an FAC content of at least 39% by weight. The metaboric acid is present in amounts sufficient to classify the calcium hypochlorite composition as a Packing Group III Division 5.1 oxidizer or as a non-Division 5.1 oxidizer, the latter being hereinafter referred to as a “Non-Oxidizer” or other similar terms. In accordance with the present invention there are further provided solid shaped articles comprising compositions of calcium hypochlorite and metaboric acid.
For purposes of this specification (other than in the operating examples) unless otherwise indicated) all numbers expressing quantities and ranges of ingredients, reaction conditions, etc, that are used in the following description and claims are to be understood as modified in all instances by the term “about”. Accordingly, unless indicated to the contrary, the numerical parameters set forth in this description and attached claims are approximations that can vary depending upon the desired properties that are sought to be obtained by the present invention. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the attached claims, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques. Further, as used in this specification and the attached claims, the singular forms “a”, “an” and “the” are intended to include plural referents, unless expressly and unequivocally limited to one referent.
Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the invention are approximations, the numerical values set forth in the specific examples are reported as precisely as possible. Any numerical value, however, inherently contains certain errors necessarily resulting from the standard deviation found in its respective testing measurement. Also, it should be understood that any numerical range recited herein is intended to include all sub-ranges subsumed therein. For example, a range of “1 to 10” is intended to include all sub-ranges between and including the recited minimum value of 1 and the recited maximum value of 10, that is having a minimum value equal to or greater than 1 and a maximum value of equal to or less than 10. Because the disclosed ranges are continuous, they include every value between the minimum and maximum values. Unless expressly indicated otherwise, the various numerical ranges specified in this application are approximations.
In accordance with regulations of the US Department of Transportation, 49 CFR §173.127(a), an “oxidizer” (Division 5.1) is defined as a material that may, generally by yielding oxygen, cause or enhance the combustion of other materials. A solid material is classed as a Division 5.1 material if, when tested in accordance with the UN Manual of Tests and Criteria, blends of it with cellulose have mean burning times less than or equal to the burning time of a 3:7 potassium bromate-cellulose mixture [49 CFR §173.127(a)(1)].
Solid Division 5.1 materials are assigned packing groups using the following criteria [49 CFR §173.127(b)]:
The particle size distribution of the particulate calcium hypochlorite materials used to prepare the compositions of the present invention can vary. The particulate size and particle size distribution of calcium hypochlorite that can be used in the present invention is not critical and thus any particulate material, e.g., from a powdery material to a granular material, can be used to prepare the compositions of the present invention. As a general guideline, particulate calcium hypochlorite typically has a principal size distribution between 100 and 6 mesh, as measured by the American Standard Test Method E11 Alternative Sieve Designation (ASTM E11 ASD); namely, the particles vary in size principally between 0.15 millimeters (mm) (0.006 inches) and 3.35 mm (0.13 inches). More commonly, the particles will have a principal size distribution between 60 mesh (0.25 mm) and 18 mesh (1.00 mm) based on ASTM E11 ASD. Further, when solid formed articles of Non-Oxidizer calcium hypochlorite compositions are prepared, one skilled in the art will typically select a particle size distribution for the calcium hypochlorite that is amenable to be compressed into the desired solid formed article, e.g., a tablet. An example of a commercially available granular calcium hypochlorite that can be used to prepare calcium hypochlorite compositions of the present invention, e.g., Non-Oxidizer compositions, is available from PPG Industries, Inc. under the trademark PITTCLOR®.
Metaboric acid can be prepared by heating boric acid at temperatures of from 110 to 130° C., e.g., in a rotary evaporator, or by heating boric acid at such temperatures under vacuum, e.g., in a vacuum oven or rotary evaporator. Since metaboric acid is hygroscopic, it should be protected from moisture present in the atmosphere to prevent it from reverting to boric acid, e.g., by use of a dry nitrogen (or other suitable chemically inert dry gas) blanket during its preparation and subsequent storage. Alternatively, the metaboric acid can be stored in a sealed container with only a small gas head space above the metaboric acid, thereby to limit the exposure of the metaboric acid to only the limited amount of moisture present in the small gas head space.
The test for oxidizing substances described in the United Nations Manual of Tests and Criteria was used to determine the oxidizer characteristics for the blends of calcium hypochlorite described in Example 6. The detailed test method is described in Section 34 of the aforementioned Manual (“Recommendations on the Transport of Dangerous Goods; Manual of Tests and Criteria”), (Revision 3), which is titled “Classification Procedures, Test Methods and Criteria Relating to Oxidizing Substances of Division 5.1”. In the test, the relative burning rates of various oxidizers (calcium hypochlorite blends in the present case) are compared to those of other known oxidizers. On the basis of this test, a blend can be defined as an oxidizer or a non-oxidizer, and if it is an oxidizer, it can be further classified into one of three Packing Groups. Tests are conducted on the blends to be evaluated mixed with dry fibrous cellulose in mixing ratios of 1:1 and 4:1, by mass, of sample to cellulose. The burn time (in seconds) is compared to the standard 3:2, 2:3 or 3:7 mixture, by mass, of potassium bromate and cellulose. The classification assigned to the sample blends are based on the test criteria described earlier for Packing Groups I, II, III or for non-Division 5.1 oxidizer materials.
Granular Pittclor® calcium hypochlorite (2.185 milligrams) was placed in an aluminum hermetic pan and scanned in a TAI DSC 2920 differential scanning calorimeter in nitrogen from 25° C. to 500° C. at a rate of 10° C./minute (DSC). The calorimeter was calibrated with indium and tin standards. The nominal nitrogen purge rate was 50 milliliters (mL)/minute. The granular calcium hypochlorite had 70% available chlorine and approximately 7% water. Similar calcium hypochlorite material is commercially available from PPG Industries, Inc under the trade name Super Zappit®.
The data obtained from the DSC showed exotherms at 201° C. and 411° C., which represented the decomposition of the calcium hypochlorite.
The procedure of Example 1 was repeated with a sample (3.505 milligrams) comprising a blend of 3 parts by weight of the calcium hypochlorite of Example 1 and 1 part by weight of metaboric acid. The data obtained from the DSC showed no strong exotherms.
The procedure of Example 1 was repeated with a sample (3.505 milligrams) comprising a blend of 3 parts by weight of the calcium hypochlorite of Example 1 and 1 part by weight of sodium metaborate dihydrate. The data obtained from the DSC showed a mild decomposition exotherm at 61° C. and a stronger decomposition exotherm at 103° C.
The procedure of Example 1 was repeated with a sample (2.140 milligrams) comprising a blend of 3 parts by weight of the calcium hypochlorite of Example 1 and 1 part by weight of sodium metaborate tetrahydrate. The data obtained from the DSC showed strong decomposition exotherms at 61° C. and at 95° C.
The data of Example 2 shows surprisingly that metaboric acid does not thermally destabilize calcium hypochlorite, as demonstrated by the lack of strong exotherms during the DSC test (even up to 500° C.) and in particular in the normal main exotherm region of approximately 200° C. or less. There was a substantial endotherm at 174° C. and a lesser endotherm at 201° C., where there would normally be a calcium hypochlorite decomposition exotherm. The endotherm that results from the condensation reaction of metaboric acid to form water vapor and boric oxide offsets the heat produced by the decomposition of calcium hypochlorite. In contrast sodium metaborate dihydrate and sodium metaborate tetrahydrate do destabilize the calcium hypochlorite. In the case of sodium metaborate dihydrate (Example 3), the composition showed an exotherm at 103° C., which is a significantly lower temperature than the first exotherm (201° C.) exhibited by calcium hypochlorite alone (Example 1). The decomposition exotherm follows an endotherm from water loss. The release of water from the sodium metaborate can contribute to the destabilization of the calcium hypochlorite. In the case of sodium metaborate tetrahydrate (Example 4), the exotherm occurred at 95° C., which is also significantly lower than the first exotherm exhibited by calcium hypochlorite alone (Example 1).
Super Shock-It™ calcium hypochlorite (28 grams), which is available from PPG Industries, Inc., having an assay of approximately 65 weight percent free available chlorine (FAC) and approximately 7 weight percent water was charged to a 2 ounce (60 mL) glass jar and sealed. The glass jar was placed in an electric oven maintained at 49° C. After 144 hours in the oven, the test sample was removed and re-analyzed. The sample was found (average of two measurements) to have lost approximately 9% FAC. Initial and final FAC values were determined using a standard method of analysis, which method comprised adding an excess of potassium iodide and acetic acid to the hypochlorite sample and titrating the liberated iodine with standardized thiosulfate. The percent loss of FAC was calculated using the following equation:
100×(Initial FAC−Final FAC)/(Initial FAC)
(In the case of the Final FAC calculation, the weight used is the weight of the calcium hypochlorite before exposure to elevated temperature. During high temperature exposure, there is some loss of weight due to formation of chlorine and water vapor. Failure to take this into account would result in underestimating the actual loss of available chlorine. This error is avoided by using the starting rather than the final weight of the sample). The lower the value of % loss of FAC, the more desirable is the composition. Part B
The procedure of Part A was repeated except that the test sample was prepared by blending 21 grams of the granular calcium hypochlorite with 7 grams of metaboric acid (Aldrich catalog #41,345-3). After 144 hours in the 49° C. oven, the test sample was found (average of two measurements) to have lost approximately 2.2% FAC.
The procedure of Part A was repeated except that the test sample was prepared by blending 21 grams of the granular calcium hypochlorite with 7 grams of sodium metaborate dihydrate (US Borax sodium metaborate 4 mole Technical, 4046). After 144 hours in the 49° C. oven, the test sample was found (average of two measurements) to have lost approximately 10.8% FAC.
The procedure of Part A was repeated except that the test sample was prepared by blending 21 grams of the granular calcium hypochlorite with 7 grams of sodium metaborate tetrahydrate (Acros organic catalog #211635000). After 144 hours in the 49° C. oven, the test sample was found (average of two measurements) to have lost approximately 9.8% FAC.
The procedure of Part A was repeated except that the test sample was prepared by blending 21 grams of the granular calcium hypochlorite with 7 grams of sodium tetraborate pentahydrate (Girvan Proteam® Supreme, 99.5%). After 144 hours in the 49° C. oven, the test sample was found (average of two measurements) to have lost approximately 11.2% FAC.
Oxidizer classifications for the calcium hypochlorite blends described in this Example were determined by comparing burn test data of test blends and reference samples, which test data was generated according to the test method and procedures detailed in Section 34 of the Recommendations on the Transport of Dangerous Goods, Manual of Tests and Criteria, (Revision 2), United Nations, New York, 1999.
The burn test procedure can be summarized as follows. A 30 cm±1 cm length of nickel-chromium wire having a diameter of 0.6±0.05 mm and a resistivity of 6.0±0.5 ohms/meter was laid in a serpentine fashion over a circular area of 38.5 square centimeters (cm2) on a 15 cm×15 cm×0.6 cm cement tile (plate or slab) having a thermal conductivity (at 0° C.) of 0.23 W.m−1.K−1. The wire was held in place by two electrically conductive screw-type contacts, located outside of the 38.5 cm2 circular area. A homogeneously mixed reference sample (30 grams) was prepared from potassium bromate (pre-dried at 65° C. for a minimum of 12 hours) and cellulose (pre-dried at 115° C. for a minimum of 4 hours to contain less than 0.5% water by dry weight) in weight ratios of 3:7 respectively. The potassium bromate and cellulose were mixed together by hand in a small glass beaker using a spatula. The potassium bromate had a purity of 99% by weight, and was obtained from Fisher Scientific (catalog number P207-250). The cellulose used was in the form of a medium fiber powder having a Whatman® advanced ion exchange cellulose designation of CF-11, available from Fisher Scientific (catalog number 05-713-004), and was stored in a desiccator.
To a 60° conical glass funnel, having a large end diameter of 70 mm and a sealed small end, was added 30 grams of the reference sample. The 38.5 cm2 circular area of the cement tile having the wire affixed to it, was placed over the 70 mm diameter opening of the filled funnel. The cement tile and funnel were together flipped over such that the funnel sat in an inverted fashion upon the block. The funnel was lifted away leaving a truncated conical pile of reference sample over the nickel-chromium wire to which was applied an alternating current sufficient to provide 150±7 watts of power. Current was applied to the wire throughout the duration of the test or for a maximum of three minutes if no burning of the sample was observed.
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manufacture and useUS20070125979 *Nov 21, 2006Jun 7, 2007Deqing LeiCoated calcium hypochlorite composition* Cited by examinerClassifications U.S. Classification252/187.28, 252/187.24, 252/187.23, 252/187.1, 252/187.27International ClassificationC01B11/06Cooperative ClassificationC11D3/3953European ClassificationC11D3/395DLegal EventsDateCodeEventDescriptionFeb 24, 2005ASAssignmentOwner name: PPG INDUSTRIES OHIO, INC., OHIOFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:PICKENS, STANLEY R.;ABRAHAM, FRED;DUBOIS, DONALD W.;REEL/FRAME:016328/0705;SIGNING DATES FROM 20050203 TO 20050207Jun 18, 2012FPAYFee paymentYear of fee payment: 4Jan 28, 2013ASAssignmentOwner name: EAGLE CONTROLLED 2 OHIO SPINCO, INC., GEORGIAFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:PPG INDUSTRIES OHIO, INC.;REEL/FRAME:029702/0982Effective date: 20130122Jan 29, 2013ASAssignmentOwner name: GENERAL ELECTRIC CAPITAL CORPORATION, CONNECTICUTFree format text: PATENT SECURITY 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