JP6374398B2 - Solid tablet unit dose oven cleaner - Google Patents

Description

  The present invention relates generally to the field of coagulation and coagulation matrices. The present invention relates to coagulation of an alkaline detergent composition free of phosphate. In particular, the present invention relates to an alkaline detergent composition that does not contain sodium hydroxide, sodium carbonate, anhydrous sodium metasilicate, preferably a phosphate comprising a polycarboxylic acid polymer as part of the coagulation matrix.

  The use of coagulation techniques and solid block detergents in corporate and industrial activities is discussed, for example, in SOLID claimed in US Reissue Patent 32,762 and US Reissue Patent 32,818 to Fernholz et al. Developed first in the POWER® brand technology. Further, a cast solid product of sodium carbonate hydrate that substantially uses a hydrated sodium carbonate material is described in Heile et al. US Pat. No. 4,595,520 and US Pat. No. 4,680,134. Which is hereby incorporated by reference in its entirety.

  More recently, attention has been directed to producing highly effective detergent materials from less caustic substances, such as soda ash, also known as sodium carbonate. Early work in the development of sodium carbonate-based detergents found that sodium carbonate hydrate-based materials often swell (ie, were dimensionally unstable) after solidification. Such swelling can interfere with packaging, dispensing, and use. The dimensional instability of the solid material is related to the unstable nature of the various hydrate forms prepared in the manufacture of the sodium carbonate solid material. Early products made with hydrated sodium carbonate typically consisted of anhydrous, 1 molar hydrate, 7 molar hydrate, 10 molar hydrate or more mixtures thereof. However, after the product is manufactured and stored at ambient temperature, the initial product hydration state shifts between hydrate forms, eg, 1 mol, 7 mol, and 10 mol hydrate, It has been found to result in dimensional instability of the block chemical. In these conventional solid form compositions, changes in moisture content and temperature cause structural and dimensional changes that can cause the solid form to fail, resulting in problems such as the solid form being incompatible with the dispenser for use. .

  Also, conventional solid alkaline detergents, particularly those intended for commercial and commercial use, generally require phosphate in their compositions. Phosphate typically serves multiple purposes for the composition, for example, controls the rate of solidification, serves to remove and float dirt, and functions as an effective hardness sequestering agent. It is described in US Pat. No. 6,258,765 that solid block functional materials can be produced using organic acetates such as carbonates, aminocarboxylates, or binders that include a phosphonate component and water. , U.S. Pat. No. 6,156,715, U.S. Pat. No. 6,150,324, and U.S. Pat. No. 6,177,392, disclosed and disclosed in the claims. Has been. Due to environmental concerns, further research has been directed to the replacement of phosphorus-containing compounds in detergents. Furthermore, the nitrilotriacetic acid (NTA) containing aminocarboxylate component used in some examples as a binder and hard sequestering agent instead of a phosphorus containing compound is believed to be a carcinogen. Thus, their use has also been reduced.

  The need for a solid, alkaline detergent solidification matrix requires a number of changes, including removal of phosphorus and / or NTA. Further modifications include coagulation matrix formulations that incorporate caustic (sodium hydroxide) in combination with less caustic such as soda ash (eg, sodium carbonate) to establish a solid, physically stable tablet composition Continue to present the difficulty of doing. It has been shown that highly caustic powders for solidification cannot consistently form stable compositions such as tablets. Therefore, it is necessary to use lower levels of sodium hydroxide in combination with other less caustic substances to formulate dimensionally stable solid compositions. These and other aspects of forming a physically stable detergent composition provide background to the present invention being provided.

  In one aspect of the present invention, a physically stable phosphate-free alkaline detergent tablet composition for a combination oven is provided.

  In one aspect of the present invention, the hydration of ash and / or hydroxide is employed to provide a physically stable, phosphate-free alkaline detergent comprising sodium carbonate, sodium hydroxide and sodium metasilicate. A method of forming a tablet is provided.

  In a further aspect of the present invention, the compositions and methods of the present invention provide a physically stable composition with durable cleaning performance, such as, for example, in a cleaning combination oven.

  One embodiment of the present invention is a solid detergent composition comprising an alkali metal hydroxide, a polycarboxylic acid polymer, sodium carbonate, water and at least one functional ingredient. According to one embodiment, when the solid detergent composition is heated to a temperature of 120 degrees Fahrenheit, the composition remains dimensionally stable and has an increase index of less than 3%. It is preferred that the composition does not contain phosphorus.

  Another embodiment includes sodium hydroxide from about 5% to about 70% by weight of the solid detergent composition, sodium carbonate from about 20% to about 90% by weight of the solid detergent composition, Among them, the polycarboxylic acid polymer is about 0.1% by mass to about 15% by mass, the solid detergent composition is about 0.1% by mass to about 10% by mass, and the solid detergent composition is about about the second alkali source. 1% by weight to about 50% by weight of a solid detergent composition comprising about 1% by weight to about 50% by weight of a chelating agent among the solid detergent compositions, wherein the detergent composition does not contain phosphorus. When heated to a temperature of 120 degrees Fahrenheit, the solid detergent composition is dimensionally stable and has an increase index of less than 3%.

  Yet another embodiment combines sodium carbonate, a second alkali source of anhydrous silicate and at least one additional functional ingredient to form a powder premix, and the powder premix is mixed with a water source. Forming a solid hydrate, and combining the solid hydrate with a source of sodium hydroxide and optionally a polycarboxylic acid polymer to form a solid detergent composition. In one aspect of the invention, the resulting solid detergent composition is phosphorus free and when heated to a temperature of 120 degrees Fahrenheit, the solid detergent composition is dimensionally stable and has an increase index of less than 3%. .

  While multiple embodiments are disclosed, still other embodiments of the present invention will become apparent to those skilled in the art from the following detailed description, which shows and describes illustrative embodiments of the invention. . Accordingly, the drawings and detailed description are to be regarded as illustrative in nature and not as restrictive.

FIG. 1 is a graph showing the dimensional stability of various exemplary formulations according to embodiments of the methods and compositions of the present invention.

FIG. 2 is a graph illustrating the compressive strength of various exemplary formulations according to embodiments of the methods and compositions of the present invention.

FIG. 3 is a graph illustrating the dimensional stability of various exemplary formulations according to embodiments of the methods and compositions of the present invention.

FIG. 4 is a graph illustrating the compressive strength of various exemplary formulations according to embodiments of the methods and compositions of the present invention.

  Various embodiments of the present invention will be described in detail with reference to the drawings, wherein like reference numerals represent like parts throughout the several views. Reference to various embodiments does not limit the scope of the invention. The figures presented herein are not limited to various embodiments in accordance with the invention, but are presented for exemplary description of the invention.

  Embodiments of the present invention are not limited to a particular solid detergent composition, as they may vary as will be understood by those skilled in the art. It should be further understood that all terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit any method or scope. . For example, as used in this specification and the appended claims, the singular forms “a”, “an”, and “the” include plural referents unless the content clearly dictates otherwise. obtain. Also, all units, prefixes, and symbols can be expressed in their SI acceptable form. Numeric ranges defined within this specification include the numbers defining the range and include each integer within the defined range.

  Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which embodiments of the invention relate. Have Many methods and materials similar, modified, or equivalent to those described herein can be used in the practice of embodiments of the present invention without undue experimentation, and preferred materials and methods are As described herein. In describing embodiments of the present invention and in the claims, the following terminology may be used in accordance with the definitions below.

  As used herein, the term “about” refers to, for example, typical measurement and liquid handling procedures used in the real world to make concentrates or use solutions; carelessness of these procedures Intended to vary in quantity that may occur due to differences in the purity of the manufacture, source, or ingredients used to make the composition or to carry out the method. Whether modified by the term “about”, the claims include equivalents to the quantities and refer to variations in quantity that may occur.

  The terms “dimensional stability” and “dimensionally stable” as used herein contemplate solid products having an increase index of less than about 3%, preferably less than about 2%.

  The terms “weight percent”, “mass percent (wt-%)”, “percent by weight”, “% by weight”, and the like, as used herein The variation of means the concentration of the substance as the mass of the substance divided by the total mass of the composition and multiplied by 100. As used herein, it is understood that “percent”, “%”, etc. are intended to be synonymous with “mass percent”, “mass%”, and the like.

  According to embodiments of the present invention, the solid composition is a pressed, extruded or cast solid composition containing a hydratable salt, an alkali active material (eg, alkali metal hydroxide) and water. The need in the prior art is overcome by providing a dimensionally stable solid composition for use in In preferred embodiments, dimensionally stable solid compositions are not used in the cast solid composition. Specifically, the composition is in any of a variety of situations where a dimensionally stable caustic-containing alkaline detergent is desired that is a product that is substantially phosphorus-free and nitrilotriacetic acid (NTA) free. It will be useful to prepare solid detergent compositions that can be used. Substantially free of phosphorus is less than about 0.5% by weight, more specifically less than about 0.1% by weight, and even more specifically about 0.000, based on the total weight of the coagulation matrix. It means a coagulation matrix having less than 01% by weight phosphorus. Free of NTA is a coagulated matrix having less than about 0.5 wt%, less than about 0.1 wt%, and often less than about 0.01 wt% NTA, based on the total weight of the solidified matrix Means. Thus, embodiments of the present invention are particularly useful in cleaning applications where it is desirable to use an environmentally friendly solid detergent.

  The coagulation matrix of the present invention can be used in any of a wide variety of situations where a dimensionally stable solid product is desired. The solidification matrix is dimensionally stable and has an appropriate solidification rate. Furthermore, the coagulation matrix may be free of phosphorus and NTA, making the coagulation matrix particularly useful in cleaning applications where it is desirable to use an environmentally friendly, solid alkaline detergent. Such applications include, but are not limited to, the use of phosphate-free alkaline detergents in combination ovens, such as those used in various food service industries. Further applications include, for example, machines employing a ware wash detergent and manual warewashing, detergency detergents, fryer boil outs, power soak sinks and Related applications, soak tanks, equipment rework, laundry and fabric cleaning and decontamination, carpet cleaning and decontamination, vehicle cleaning and care applications, surface cleaning and decontamination, kitchen and bathing It may include cleaning and decontamination, floor cleaning and decontamination, in-place cleaning operations, general purpose cleaning and decontamination, and / or industrial or household detergents. A suitable method for preparing a solid detergent composition using a coagulation matrix is also provided.

Solidification matrix and solid detergent composition The solidification matrix generally comprises an alkali source of alkali metal hydroxide, a hydratable salt such as sodium carbonate (soda ash), a polycarboxylic acid polymer and water to form the solid composition. Includes water charge. The solidification matrix may further comprise a chelating agent, a corrosion inhibitor, an additional water conditioner and / or an additional alkaline source. The coagulation matrix comprises, consists of, consists of alkali metal hydroxides, hydratable salts, polycarboxylic acid polymers, chelating agents, additional alkali and / or corrosion inhibitor sources and / or water charges, and And / or can consist essentially of these.

  Suitable component concentrations for the coagulation matrix include alkali metal hydroxide alkali content of about 0.1% to about 90%, polycarboxylic acid polymer of about 0.1% to about 15%, and water of about 0.1%. The range is from 0.1% to about 25% by weight and sodium carbonate from about 20% to about 90% by weight. Particularly suitable component concentrations for the coagulation matrix are alkali metal hydroxide alkali content of about 5% to about 70%, polycarboxylic acid polymer of 1% to about 10%, and water of about 0.1%. % To about 10% by weight, and sodium carbonate in the range of about 25% to about 90% by weight. More particularly suitable component concentrations for the coagulation matrix are alkali metal hydroxides having an alkali content of about 10% to about 50% by weight, a polycarboxylic acid polymer of 2.5% to about 10% by weight, and water of about 1 Mass% to about 5 mass% and sodium carbonate in the range of about 30 mass% to about 70 mass%. Surprisingly, according to the invention, a dimensionally stable solid composition is at least 30% or more, preferably at least 40% or more, or at least 50% or more. It has a content of up to many alkali metal hydroxides (eg sodium hydroxide), overcoming significant limitations in the art.

  In a further aspect of the present invention, the concentration of the coagulation matrix component is about 0.1% to 50% by weight of a chelating agent such as sodium gluconate and 0.2% of the second alkali source and / or corrosion inhibitor. Furthermore, the range of 1 mass%-50 mass% is included. Particularly suitable coagulation matrix component concentrations range from about 1% to 50% by weight of the chelating agent and from 1% to 50% by weight of the second alkali source and / or corrosion inhibitor. More particularly suitable coagulation matrix component concentrations range from about 5% to 25% by weight of the chelating agent and from 1% to 20% by weight of the second alkali source and / or corrosion inhibitor. Those skilled in the art will recognize other suitable component concentration ranges to obtain comparable properties of the coagulation matrix. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

Alkali Source The solid detergent composition includes one or more effective amounts of alkali source to provide effective cleaning of the substrate and to improve the soil removal performance of the solid detergent composition. Preferably, the alkali source is an alkali metal hydroxide and is provided in an amount effective to improve substrate cleaning and soil removal. The compositions of the present invention comprise an alkali source in an amount of at least about 1%, at least about 5%, or at least about 10% by weight. In preferred embodiments, the alkali source is about 1% to about 90%, about 5% to about 70%, about 10% to about 50%, and most preferably, of the total weight of the solid detergent composition. Constitutes about 20% to about 40% by weight.

  An effective amount of alkaline source should be considered as an amount that provides a use composition having a pH of at least about 8, preferably at least about 10, and more preferably at least about 12. If the use composition has a pH of about 8 to about 10, it can be considered weakly alkaline, and if the pH is greater than about 12, the use composition can be considered caustic.

  Examples of suitable alkali sources for solid detergent compositions include, but are not limited to, alkali metal hydroxides. Exemplary alkali metal hydroxides that can be used include, but are not limited to, sodium, lithium, or potassium hydroxide. The alkali metal hydroxide can be added to the composition in a form known in the art, including solid beads, a form dissolved in an aqueous solution, or a combination thereof. The alkali metal hydroxide is about 12-100 U. S. Commercially available as granulated solids or beaded solids mixed with particle sizes in the mesh range, or as aqueous solutions, for example, as 45% and 50% by weight solutions. The alkali metal hydroxide according to the present invention is preferably added in the form of granular solid or beads.

Hydrateable Salt The solid detergent composition according to the present invention comprises at least one hydratable salt. In one embodiment, the hydratable salt is sodium carbonate (aka soda ash or ash) and / or potassium carbonate (aka potash). In a preferred embodiment, the hydratable salt is sodium carbonate, excluding potassium carbonate. The hydratable salt is a hydratable salt, such as about 20% to about 90%, preferably about 25% to about 90%, and more preferably about 30% to about 90% by weight of sodium carbonate. Provided in the range of 70% by weight. Those skilled in the art will recognize other suitable component concentration ranges to obtain comparable properties of the coagulation matrix.

  In other embodiments, the hydratable salt may be combined with other coagulants. For example, hydratable salts may be used with additional coagulants that are inherently inorganic and may optionally serve as an alkali source. In certain embodiments, the second coagulant includes, but is not limited to, additional alkali metal hydroxides, anhydrous sodium carbonate, anhydrous sodium sulfate, anhydrous sodium acetate, and other known hydratable compounds. Or a combination thereof. According to a preferred embodiment, the second hydratable salt comprises sodium metasilicate and / or anhydrous sodium metasilicate. The amount of second coagulant needed to achieve coagulation depends on several factors including the exact coagulant used, the amount of water in the composition, and the hydration capacity of other detergent ingredients. In certain embodiments, the second coagulant can also serve as an additional alkali source.

Polycarboxylic Acid Polymers The solid alkaline detergent composition according to the present invention comprises a polycarboxylic acid polymer or a salt or derivative thereof. As referred to herein, reference to polycarboxylic acid polymers further includes their salts or derivatives that are also suitable polymers for use in solid alkaline detergent compositions according to the present invention. Examples of particularly suitable polycarboxylic acid polymers include, but are not limited to, polyacrylic acid polymers, polyacrylic acid polymers modified with fatty acid end groups ("modified polyacrylic acid polymers"), polymaleic acid Includes polymers and combinations of these polymeric materials. Each salt of the polycarboxylic acid polymers can be further employed in a solid alkaline detergent composition.

  Non-limiting examples of polycarboxylic acid polymer salts include polyacrylic acid salts and derivatives such as water-soluble acrylic polymers. Such polymers include, but are not limited to, polyacrylic acid, polymethacrylic acid, acrylic acid, acrylic acid-methacrylic acid copolymer, polymaleic acid, hydrolyzed polyacrylamide, hydrolyzed methacrylamide, Hydrolyzed acrylamide-methacrylamide copolymer, hydrolyzed polyacrylonitrile, hydrolyzed polymethacrylonitrile, hydrolyzed acrylonitrile methacrylonitrile copolymer, etc., or combinations or copolymers thereof Including. Water-soluble or partial salts of these polymers, such as their respective alkali metal (eg, sodium, potassium, or combinations thereof) or ammonium salts can also be used in accordance with the present invention.

  Examples of particularly suitable polyacrylic acid polymers and modified polyacrylic acid polymers and salts and derivatives thereof include those having a molecular weight of about 1,000 to about 100,000. Examples of more particularly suitable polymaleic acid polymers and salts and derivatives thereof include those having a molecular weight of about 500 to about 5,000. Examples of particularly suitable commercially available polyacrylic acid polymers and salts and derivatives thereof include, but are not limited to, Acusol 445ND available from Rohm & Haas LLC, Philadelphia, PA. Examples of particularly suitable commercially available modified polyacrylic acid polymers include, but are not limited to, Alcosperse 325 available from Alco Chemical, Chattanooga, TN. Examples of particularly suitable commercially available polymaleic acid polymers include, but are not limited to, Belclene 200 available from Houghton Chemical Corporation, Boston, MA and Aquature AR-801 available from Alco Chemical, Chattanooga, TN. .

  In one embodiment, the coagulation matrix of the present invention comprises at least one polyacrylic acid polymer or salt or derivative thereof. For example, the coagulation matrix may comprise about 0.1 wt% to 15 wt% polyacrylic acid polymer, more specifically about 0.5 wt% to 15 wt%, and about 0.1 wt% to 10 wt%. It may contain about 1% to 10% by weight, more specifically about 2.5% to 10% by weight. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

  In another embodiment, the coagulation matrix can include a polymaleic acid polymer and at least two polyacrylic acid polymers having different molecular weights. In a further embodiment, the coagulation matrix comprises at least one carboxylate salt in addition to at least one polycarboxylic acid polymer. Suitable carboxylates include, for example, linear saturated carboxylates such as acetic acid, gluconic acid, malic acid, succinic acid, glutaric acid, adipic acid, tartaric acid, citric acid, or combinations thereof. In one example, the coagulation includes about 0.1% to 10% by weight carboxylate, such as citrate.

Water According to aspects of the present invention, water may be added to the coagulation matrix independently and / or provided in the coagulation matrix as a result of its presence in the aqueous material added to the detergent composition. Good. Preferably, the second alkali source (eg, silicate or metasilicate) is provided as anhydrous silicate so that no water is introduced into the coagulation matrix. However, the remaining ingredients added to the detergent composition may contain water or may be prepared in an aqueous premix available for reaction with one or more ingredients of the coagulation matrix. Water is introduced into the coagulation matrix to provide a coagulation matrix having the desired cohesive strength or compressibility and the desired rate of coagulation (eg, hydroxide and / or ash hydration according to embodiments of the present invention). I will provide a. In addition, when it is desired to form the concentrate as a solid, the aqueous medium is expected to help the coagulation process. The water may also be provided as deionized water or as soft water.

  The amount of water in the resulting solid detergent composition will depend on the molding method (eg, processing molding technique) used for the solid detergent composition. When the methods and compositions of the present invention are not preferred for use in casting (coagulation occurring in a container), a small amount of water is used. The use of molding techniques involves a relatively small amount of water for coagulation compared to casting techniques. When preparing a solid detergent composition by molding techniques, the water is about 1% to about 25%, especially about 1% to about 20%, and more specifically about 2% to about 10%. It can be present in the mass% range. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

  The coagulation matrix may be free of phosphorus and / or nitrilotriacetic acid (NTA) to make the solid detergent composition more environmentally beneficial. Free of phosphorus is less than about 0.5 wt%, more specifically less than about 0.1 wt%, and even more specifically less than about 0.01 wt%, based on the total weight of the coagulation matrix. Means a coagulation matrix having Free of NTA refers to a coagulated matrix having less than about 0.5 wt%, less than about 0.1 wt%, and often less than about 0.01 wt% NTA, based on the total weight of the solidified matrix. Means. If the coagulation matrix does not contain NTA, the coagulation matrix and the resulting solid detergent composition are also compatible with chlorine, which functions as an anti-redeposition and soil removal agent.

Additional Functional Materials The components of the coagulation matrix can be mixed with various functional components used to form a solid detergent composition. In some embodiments, for example, in an aspect having little or no additional functional material disposed therein, alkali metal hydroxide, second alkali source, chelating agent, polycarboxylic acid polymer, water, And a coagulation matrix comprising sodium carbonate constitutes a majority or even substantially all of the total weight of the detergent composition. In these embodiments, the concentration ranges of ingredients provided above for the coagulation matrix represent those same ingredient ranges in the detergent composition. For example, such a composition comprises about 5% to 70% by weight alkali metal hydroxide, 0.1% to 15% by weight polycarboxylic acid polymer, about 0.1% to about 10% by weight. Of water, about 20% to 90% sodium carbonate, about 1% to 50% by weight of a second alkali source, and about 1% to 50% by weight of a chelating agent, The balance contains additional functional ingredients. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

  The functional material provides the desired properties and functions for the solid detergent composition. For the purposes of this application, the term “functional material” includes materials that provide beneficial properties for a particular use when used and / or dispersed or dissolved in a concentrated liquid, eg, an aqueous solution. Some specific examples of functional materials are discussed in more detail below, and the specific materials considered are given through examples only, but a wide variety of other functional materials may be used. It is considered. For example, many of the functional materials discussed below relate to materials used in cleaning and / or decontamination applications. However, other embodiments may include functional materials for use in other applications.

Second Alkaline Source The solid detergent composition provides an alkalinity and / or enhances the cleaning of the substrate and / or improves the soil removal performance of the solid detergent composition by an effective amount of one or more. Many secondary alkali sources can be included. Similar to the alkali metal hydroxide alkali source, the second alkali source may be provided in the form of a concentrate.

  Examples of suitable second alkali sources for the solid detergent composition include, but are not limited to, alkali metal carbonates such as sodium or potassium carbonate, bicarbonate, sesquicarbonate, and mixtures thereof; Metal silicates such as sodium or potassium silicate or metasilicate, and mixtures thereof; metal borates such as sodium or potassium borate, and mixtures thereof; and ethanolamines and amines; And mixtures thereof. Such second alkaline agents are generally available in either aqueous or powder form, any of which are useful for formulating the solid detergent composition of the present invention. According to a preferred embodiment of the present invention, the second alkaline agent is provided in solid form.

  In one aspect, silicates are preferably used as the second alkali source. Silicates are known for their conventional benefits of corrosion inhibition and / or anti-redeposition effects in addition to providing alkalinity. In one aspect of the invention, the second alkali source of silicate is not provided in an amount sufficient for metal protection (ie, corrosion inhibition) as a result of the solidification composition comprising an alkali metal hydroxide component. Exemplary silicates include, but are not limited to, sodium silicate and potassium silicate. As mentioned herein, the silicates can further comprise metasilicates (eg, potassium or sodium metasilicates). Silicates and / or metasilicates can be provided as powder, particulate or granular silicates and / or metasilicates. Also, the silicates and / or metasilicates can be anhydrous or contain water of hydration. In a preferred embodiment of the invention, the silicates and / or metasilicates are anhydrous.

  In some embodiments, the second alkali source is from about 0.1% to about 50%, from about 0.5% to about 50%, from about 1% by weight to the total weight of the solid detergent composition. Provided in amounts of about 50%, about 1% to about 25%, and about 5% to about 15% by weight. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

Surfactant The solid detergent composition can comprise at least one cleaning agent comprising a surfactant or surfactant system. A variety of surfactants are used in solid detergent compositions, including but not limited to anionic, nonionic, cationic, and zwitterionic surfactants. Surfactants are an optional component of the solid detergent composition and can be excluded from the concentrate. Exemplary surfactants that can be used are commercially available from a number of sources. For a description of surfactants, see Kirk-Othmer, Encyclopedia of Chemical Technology, Third Edition, Volume 8, pages 900-912, which is incorporated herein by reference in its entirety. If the solid detergent composition includes a cleaning agent, the cleaning agent is provided in an amount effective to provide the desired level of cleaning. The solid detergent composition, when provided as a concentrate, is about 0.05% to about 20%, about 0.5% to about 15%, about 1% to about 15%, about 1%. Detergents can be included in the range of from 5% to about 10% and from about 2% to about 8% by weight. Further exemplary ranges of surfactants in the concentrate include from about 0.5% to about 8%, and from about 1% to about 5% by weight. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

  Examples of anionic surfactants useful in solid detergent compositions include, but are not limited to, carboxyl carboxylates and polyalkoxycarboxylates, alcohol ethoxylate carboxylates, nonylphenol ethoxylate carboxylates and the like. Sulfonates such as alkyl sulfonates, alkylbenzene sulfonates, alkylaryl sulfonates, sulfonated fatty acid esters; sulfated alcohols, sulfated alcohol ethoxylates, sulfated alkylphenols, alkyl sulfates, sulfosuccinate And sulfates such as alkyl ether sulfates. Typical anionic surfactants include, but are not limited to, sodium alkyl aryl sulfonates, α-olefin sulfonates, and fatty alcohol sulfates.

  Examples of nonionic surfactants useful in solid detergent compositions include, but are not limited to, those having a polyalkylene oxide polymer as part of the surfactant molecule. Such nonionic surfactants include, but are not limited to, chlorine-, benzyl-, methyl-, ethyl-, propyl-, butyl- and other similar alkyl-capped polyethylenes of fatty alcohols. Nonionic substances not containing polyalkylene oxide such as alkyl polyglycosides; sorbitan and sucrose esters and ethoxylates thereof; alkoxylated amines such as alkoxylated ethylenediamine; alcohol ethoxylate propoxylates; Alcohol alkoxylates such as alcohol propoxylates, alcohol propoxylate ethoxylate propoxylates, alcohol ethoxylate butoxylates; nonylphenol ethoxylate, polyoxyethylene Recall ether; Carboxylic acid esters such as glycerol esters, polyoxyethylene esters, ethoxylation and glycol esters of fatty acids; Carboxylic acids such as diethanolamine condensates, monoalkanolamine condensates, polyoxyethylene fatty acid amides Amides; and polyalkylene oxide block copolymers. Examples of commercially available ethylene oxide / propylene oxide block copolymers include, but are not limited to, PLURONIC®, available from BASF Corporation, Florham Park, NJ. Examples of commercially available silicone surfactants include, but are not limited to, ABIL® B8852 available from Goldschmidt Chemical Corporation, Hopewell, VA.

Examples of cationic surfactants that can be used in solid detergent compositions include, but are not limited to, primary, secondary and tertiary monoamines having _C18 alkyl or alkenyl chains, ethoxyl. Alkylamines, amines such as ethylenediamine alkoxylates, imidazoles such as 1- (2-hydroxyethyl) -2-imidazoline, 2-alkyl-1- (2-hydroxyethyl) -2-imidazoline; and Quaternary ammonium salts such as n-alkyl (C ₁₂ -C ₁₈ ) dimethylbenzylammonium chloride, n-tetradecyldimethylbenzylammonium chloride monohydrate, and naphthylene-substituted dimethyl-1-naphthylmethylammonium chloride Alkyl such as quaternary ammonium chloride Including quaternary ammonium chloride surfactants. Cationic surfactants can be used to provide disinfecting properties.

  Examples of zwitterionic surfactants that can be used in solid detergent compositions include, but are not limited to, betaines, imidazolines, and propionates.

  The solid detergent composition is intended for use in an automatic dish or dishwasher or combination oven, so if any surfactant is used, the selected surfactant is the dish or dishwasher Or when used in a combination oven, it may provide an acceptable level of foaming. Solid detergent compositions for use in automatic dish or dishwashers are generally considered to be low foaming compositions. Low foaming surfactants that provide the desired level of detergent activity are advantageous in environments such as dishwashers where the presence of large amounts of foam can be a problem. In addition to selecting a low foaming surfactant, antifoaming agents can also be utilized to reduce foam generation. Accordingly, a surfactant that is considered to be a low foaming surfactant can be used. Other surfactants can also be used with antifoam agents to control the level of foaming.

Chelating agents, builders and / or water conditioners Solid detergent compositions are also referred to as chelating agents or sequestering agents (eg, builders), including but not limited to aminocarboxylic acids, or polyacrylates, One or more building agents can be included. In general, chelating agents are molecules capable of coordinating (ie, binding) metal ions commonly found in natural water and prevent the metal ions from interfering with the action of other detersive components of the cleaning composition. . Preferred levels of addition of builders, which can also be chelating agents or sequestering agents, are from about 0.1% to about 70%, from about 1% to about 60%, or from about 1.5% to about 50%. %. When the solid detergent is provided as a concentrate, the concentrate includes from about 1% to about 60%, from about 3% to about 50%, and from about 6% to about 45% builder. Can do. Additional ranges of builders include about 3% to about 20%, about 6% to about 15%, about 25% to about 50%, and about 35% to about 45% by weight. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

  In preferred embodiments, the chelating agent (eg, sodium gluconate) is about 0.1% to about 50%, about 0.5% to about 50%, about 1% by weight of the total weight of the solid detergent composition. Provided in an amount of from about 50% to about 50%, from about 1% to about 25%, and from about 5% to about 25% by weight. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

  Examples of preferred chelating agents for use in non-phosphate alkaline detergent compositions include carboxylic acid salts such as citrate, tartrate or gluconate. In a preferred embodiment, sodium gluconate is used as a chelating agent for solid alkaline detergent compositions.

  The solid detergent composition can include a non-phosphorous builder. The various components may contain trace amounts of phosphorus, but compositions that are believed to be free of phosphorus generally include phosphate or phosphonate builder or chelate components as intentionally added components. Not included. Carboxylates such as citrate, tartrate or gluconate are suitable. Useful aminocarboxylic acid materials with little or no NTA include, but are not limited to, N-hydroxyethylaminodiacetic acid, ethylenediaminetetraacetic acid (EDTA), hydroxyethylenediaminetetraacetic acid, diethylenetriaminepentaacetic acid, N-hydroxyethyl- Includes ethylenediaminetriacetic acid (HEDTA), diethylenetriaminepentaacetic acid (DTPA), and other similar acids with carboxylic acid substituents and amino groups.

The water quality adjusting polymer can be used as a builder containing no phosphorus. Exemplary water conditioning polymers include, but are not limited to, polycarboxylates. Exemplary polycarboxylates that can be used as builders and / or water conditioning polymers include, but are not limited to, those having pendant carboxylate (—CO ₂ —) groups such as polyacrylic acid and maleic acid, maleic acid / Olefin copolymer, sulfonated copolymer or terpolymer, acrylic acid / maleic acid copolymer, polymethacrylic acid, acrylic acid methacrylic acid copolymer, hydrolyzed polyacrylamide, hydrolyzed polymethacrylamide, hydrolyzed polyamide-methacrylic Including amide copolymers, hydrolyzed polyacrylonitrile, hydrolyzed polymethacrylonitrile, and hydrolyzed acrylonitrile-methacrylonitrile copolymers. For further description of chelating / sequestering agents, see Kirk-Othmer, Encyclopedia of Chemical Technology, Third Edition, Volume 5, pages 339-366 and Volumes 23, pages 319-320 of this disclosure. See Import). These materials can also be used at substoichiometric levels to function as crystal modifiers.

Curing Agent The solid detergent composition can also include a curing agent in addition to or in the form of a builder. The curing agent is a compound or system of compounds, organic or inorganic that contributes significantly to the uniform solidification of the composition. Preferably, the curing agent is compatible with a detergent comprising an active alkali of sodium hydroxide, and other active ingredients of the composition, and provides an effective amount of hardness and / or water solubility to the processed composition. be able to. The hardener should be able to form a homogeneous matrix with the detergent and other ingredients when mixed and solidified to provide uniform dissolution of the detergent from the solid detergent composition in use. .

  The amount of hardener contained in the solid detergent composition is not limited to these, but includes the type of solid detergent composition to be prepared, the components of the solid detergent composition, the intended use of the composition, and the time spent during use. The amount of dispensing solution applied to the solid composition, the temperature of the dispensing solution, the hardness of the dispensing solution, the physical size of the solid detergent composition, the concentration of other ingredients, and the concentration of the detergent in the composition Will vary depending on factors including The amount of hardener contained in the solid detergent composition is a mixture of the cleaning agent and the other components of the composition, which is a homogeneous mixture under continuous mixing conditions and at or below the melting temperature of the hardener. It is preferable that it is effective to produce.

  Mixing is discontinued and the mixture is within the range of less than about 1 minute, or within the range of about 1 minute to about 3 hours, particularly less than about 2 minutes to about 2 hours, and particularly less than about 5 minutes to about 1 hour. A matrix having a cleaning agent and other components that can be cured to a solid form at ambient temperatures of about 30 ° C. to about 50 ° C., particularly about 35 ° C. to about 45 ° C. after being dispensed from the mixing system. Is preferably formed. A minimal amount of heat from an external source can be applied to the mixture to facilitate processing of the mixture. The amount of hardener contained in the solid detergent composition was processed when placed in an aqueous medium to achieve the desired dispensing rate of the cleaning agent from the composition solidified during use. It is preferably effective to provide the desired hardness and the desired controlled dissolution rate of the composition.

The curing agent may be an organic or inorganic curing agent. According to one aspect of the present invention, it is preferred that the organic curing agent is not a polyethylene glycol (PEG) compound, as shown in Examples 10-23 of the present invention. Examples of polyethylene glycols include, but are not limited to, those of the general formula H (OCH ₂ CH ₂ ) _n OH, where n is greater than 15, especially from about 30 to about 1700 having various molecular weights. Contains solid polyethylene glycols. More preferably, the curing agent is not urea and / or urea particles.

  Preferred inorganic hardeners are hydratable inorganic salts, including but not limited to sulfates and bicarbonates. The inorganic curing agent is present at a concentration of up to about 50% by weight, in particular from about 1% to about 25% by weight, and more specifically from about 5% to about 15% by weight. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

Bleaching agents Suitable for use in solid detergent compositions for lightening or whitening substrates are typically Cl ₂ , Br under the conditions encountered during the washing process. _2, -OCl ^- and the like bleaching compounds capable of liberating an active halogen species ^- and / or -OBr. Suitable bleaching agents for use in the solid detergent composition include, but are not limited to, chlorine-containing compounds such as chlorines, hypochlorites, or chloramines. Exemplary halogen releasing compounds include, but are not limited to, alkali metal dichloroisocyanurates, chlorinated trisodium phosphate, alkali metal hypochlorites, monochloramine, and dichloramine. The encapsulated chlorine source can also be used to increase the stability of the chlorine source in the composition (eg, US Pat. No. 4,618,914 and US Pat. No. 4,830,773) The disclosure of which is incorporated herein by reference). Bleaching agents also have hydrogen peroxide, perborate, sodium carbonate hydrogen peroxide, potassium permonosulfate, and sodium perborate mono- and tetrahydrate with and without activators such as tetraacetylethylenediamine. It may be a peroxide or active oxygen source.

  When the concentrate includes a bleaching agent, it is from about 0.1% to about 60%, from about 1% to about 20%, from about 3% to about 8%, and from about 3% to about It can be included in an amount of 6% by weight. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

Filler The solid detergent composition may contain an effective amount of detergent filler that does not function as a cleaning agent by itself, but cooperates with the cleaning agent to increase the overall cleaning ability of the composition. Examples of suitable detergent fillers for use in the cleaning compositions of the present application include, but are not limited to sodium sulfate and sodium chloride. When the concentrate includes a detergent filler, it can be included in an amount of up to about 50%, about 1% to about 30%, or about 1.5% to about 25% by weight. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

Antifoaming agents Antifoaming agents for reducing foam stability may also be included in the dishwashing composition. Examples of antifoaming agents include ethylene oxide / propylene block copolymers such as those available under the name Pluronic N-3; silicone compounds such as silica dispersed in polydimethylsiloxane, polydimethylsiloxane, and Abil B9952 Functionalized polydimethylsiloxanes such as those available under the name of: fatty amides, hydrocarbon waxes, fatty acids, fatty esters, fatty alcohols, fatty acid soaps, ethoxylates, mineral oils, Including but not limited to polyethylene glycol esters and alkyl phosphate esters such as monostearyl phosphate.

  Defoaming agents are discussed in, for example, Martin et al. US Pat. No. 3,048,548, Brunelle et al. US Pat. No. 3,334,147, and Rue et al. US Pat. No. 242 (the disclosures of which are incorporated herein by reference). When the concentrate includes an antifoaming agent, the antifoaming agent is about 0.0001% to about 10%, about 0.001% to about 5%, or about 0.01% to about 1.% by weight. It can be provided in an amount of 0% by weight. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

Anti-redeposition agent The solid detergent composition promotes sustained suspension of soil in the cleaning solution and prevents re-deposition to prevent the removed soil from redepositing on the substrate being cleaned. An agent can be included. Examples of suitable anti-redeposition agents include, but are not limited to, polyacrylates, styrene maleic anhydride copolymers, cellulose derivatives such as hydroxyethyl cellulose, hydroxypropyl cellulose and carboxymethyl cellulose. Where the concentrate includes an anti-redeposition agent, the anti-redeposition agent may be included in amounts of about 0.5% to about 10%, and about 1% to about 5%. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

Stabilizer The solid detergent composition can also include a stabilizer. Examples of suitable stabilizers include, but are not limited to, borates, calcium / magnesium ions, propylene glycol, and mixtures thereof. The concentrate need not include a stabilizer, but if the concentrate includes a stabilizer, it can be included in an amount that provides the desired level of stability of the concentrate. Exemplary ranges of stabilizers include up to about 20%, about 0.5% to about 15%, and about 2% to about 10% by weight. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

Dispersants The solid detergent composition can also include a dispersant. Examples of suitable dispersants that may be used in the solid detergent composition include, but are not limited to, maleic acid / olefin copolymers, polyacrylic acid, and mixtures thereof. The concentrate need not include a dispersant, but if a dispersant is included, it can be included in an amount that provides the desired dispersion characteristics. Exemplary ranges of dispersants in the concentrate can be up to about 20%, from about 0.5% to about 15%, and from about 2% to about 9%. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

Enzymes Enzymes that can be included in the solid detergent composition include enzymes that help remove starch and / or protein stains. Exemplary enzyme types include, but are not limited to, proteases, α-amylases, and mixtures thereof. Exemplary proteases that can be used are derived from Bacillus licheniformix, Bacillus lenus, Bacillus alcalophilus, and Bacillus amyloliquefacins. Including, but not limited to. Exemplary α-amylases include Bacillus subtiles, Bacillus amyloliquefaceins, and Bacillus licheniformis. The concentrate need not contain an enzyme, but if the concentrate contains an enzyme, it can be included in an amount that provides the desired enzyme activity when the solid detergent composition is provided as a use composition. . Exemplary ranges of enzymes in the concentrate include up to about 15%, about 0.5% to about 10%, and about 1% to about 5% by weight. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

Glass and Metal Corrosion Inhibitors The solid detergent composition may comprise a metal corrosion inhibitor in an amount of up to about 50 wt%, about 1 wt% to about 40 wt%, or about 3 wt% to about 30 wt%. it can. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

  Corrosion Inhibitor provides a use solution that exhibits a glass corrosion and / or etch rate that is less than the rate of glass corrosion and / or etch for a use solution that is otherwise identical except for the absence of a corrosion inhibitor. Contained in the solid detergent composition in an amount sufficient to do so. It is anticipated that the use solution may contain at least about 1 part per million (ppm) corrosion inhibitor to provide the desired corrosion inhibiting properties. It is expected that higher amounts of corrosion inhibitors can be used in the use solution without deleterious effects. In some respects, the effects of increased corrosion and / or etch resistance additives with increasing corrosion inhibitor concentration are lost, and additional corrosion inhibitors simply increase the cost of using the solid detergent composition. Expected to be deaf. The use solution can include about 6 ppm to about 300 ppm of a corrosion inhibitor, and about 20 ppm to about 200 ppm of a corrosion inhibitor. Examples of suitable corrosion inhibitors include, but are not limited to, a combination of an aluminum ion source and a zinc ion source, and alkali metal silicates or hydrates thereof.

  The corrosion inhibitor can be said to be a combination of an aluminum ion source and a zinc ion source. When the solid detergent composition is provided in the form of a use solution, the aluminum ion source and the zinc ion source provide aluminum ions and zinc ions, respectively. The amount of corrosion inhibitor is calculated based on the total amount of aluminum ion source and zinc ion source. Anything that provides aluminum ions in the use solution can be referred to as an aluminum ion source, and anything that provides zinc ions when provided in the use solution can be referred to as a zinc ion source. It is not necessary for the aluminum ion source and / or zinc ion source to react to produce aluminum ions and / or zinc ions. Aluminum ions can be considered an aluminum ion source, and zinc ions can be considered a zinc ion source. The aluminum ion source and zinc ion source can be provided as organic salts, inorganic salts, and mixtures thereof. Exemplary aluminum ion sources include sodium aluminate, aluminum bromide, aluminum chlorate, aluminum chloride, aluminum iodide, aluminum nitrate, aluminum sulfate, aluminum acetate, aluminum formate, aluminum tartrate, aluminum lactate, aluminum oleate, Including but not limited to aluminum salts such as aluminum bromate, aluminum borate, potassium aluminum sulfate, aluminum zinc sulfate, and aluminum phosphate. Exemplary zinc ion sources include zinc chloride, zinc sulfate, zinc nitrate, zinc iodide, zinc thiocyanate, zinc fluorosilicate, zinc dichromate, zinc chlorate, sodium zincate, zinc gluconate, zinc acetate, Including, but not limited to, zinc salts such as zinc benzoate, zinc citrate, zinc lactate, zinc formate, zinc bromate, zinc bromide, zinc fluoride, zinc silicofluoride, and zinc salicylate.

  Applicants have reduced corrosion and / or etching of glassware and ceramics by controlling the ratio of aluminum ions to zinc ions in the use solution compared to the use of either component alone. I found out that it could be offered. That is, the combination of aluminum ions and zinc ions can provide a synergistic effect in reducing corrosion and / or etching. The ratio of the aluminum ion source to the zinc ion source can be controlled to provide a synergistic effect. Generally, the weight ratio of aluminum ions to zinc ions in the use solution can be at least about 6: 1, can be less than about 1:20, and can be from about 2: 1 to about 1:15. .

Effective amounts of alkali metal silicates or hydrates thereof can be used in the compositions and methods of the present invention to form stable solid detergent compositions with metal protection capabilities. The silicates used in the compositions of the present invention are those commonly used in solid detergent formulations. For example, typical alkali metal silicates are anhydrous or preferably hydrated water (about 5% to about 25%, especially about 15% to about 20% hydrated water). These are powdered, particulate or granular silicates. These silicates are preferably sodium silicate and have a Na ₂ O: SiO ₂ ratio of about 1: 1 to about 1: 5, respectively, and typically about 5% to about Contains water available in an amount of 25% by weight. Generally, the silicate is from about 1: 1 to about 1: 3.75, in particular from about 1: 1.5 to about 1: 3.75 and most specifically from about 1: 1.5 to about 1. Has a Na ₂ O: SiO ₂ ratio of 2.5. Most preferred are silicates having a Na ₂ O: SiO ₂ ratio of about 1: 2 and about 16% to about 22% by weight water of hydration. For example, such silicates are available from PQ Corporation, Valley Forge, PA in powder form as GD silicate and in granular form as Britesil H-20. These ratios may be obtained with a single silicate composition or with a combination of silicates resulting in a preferred ratio by combination. Hydrated silicates with preferred ratios (Na ₂ O: SiO ₂ ratio of about 1: 1.5 to about 1: 2.5) provide optimal metal protection and rapidly form solid detergents Has been found. Hydrated silicates are preferred.

  Silicates are included in solid detergent compositions and can provide metal protection, but are further known to provide additional functions as alkaline and anti-redeposition agents. Exemplary silicates include, but are not limited to, sodium silicate and potassium silicate. Solid detergent compositions can be provided without silicates, but if silicates are included, they can be included in an amount that provides the desired metal protection. The concentrate can include silicates in an amount of at least about 1%, at least about 5%, at least about 10%, and at least about 15% by weight. Further, to provide sufficient room for other components in the concentrate, the silicate component is less than about 35 wt%, less than about 25 wt%, less than about 20 wt%, and about 15 wt%. May be provided at less than levels. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

Perfumes and dyes Various dyes, odorants including perfumes, and other aesthetic enhancing agents may also be included in the composition. Suitable dyes that can be included to modify the appearance of the composition are Direct Blue 86 available from Mac Dye-Chem Industries, Ahmedabad, India; Feast available from Mobay Chemical Corporation, Pittsburgh, PA; Acid Orange 7 available from the American Cyanamid Company, Wayne, NJ; Basic Violet 10 available from Sandoz, Princeton, NJ; available from Sando Blue / Acid Blue 182 available from Chemo, Gem 23; Sigma Chem cal, St. Acid Yellow 17 available from Louis, MO; Sap Green and Metalil Yellow available from Keystone Analine and Chemical, Chicago, IL; Available from Emerton Hilton Davis, LLC, CincinitB Hisol Fast Red and Fluorescein available from the Color and Chemical Company, Newark, NJ; and Ciba Specialty Chemicals Corporation, Greenboro, NC Acid Green 25, including but not limited to.

  Perfumes or perfumes that may be included in the composition include, but are not limited to, terpenoids such as citronellol, aldehydes such as amylcinnamaldehyde, jasmine such as ClS-jasmine or jasmal, and vanillin.

Flow aids Various flow aids may also be included in the composition. Flow aids may further be referred to as carriers and / or glidants and are generally known to improve the processing of compositions such as solid detergent compositions according to the present invention. Suitable ingredients for improving the flowability of the homogeneous powder component according to the present invention may include, for example, inorganic or organic agents. According to one aspect, inorganic agents are preferred, including, for example, silicas, borates, acetates, sulfates, and the like. For example, silicas containing precipitated or fumed forms (e.g. Sipernat (R), Aerosil (R), CAB-O-SIL (R)) can be employed, e.g., commercially available from Evonik Industries .

Production and Use Without being limited to a particular theory of the present invention, the actual coagulation mechanism is based on the hydration reaction of hydroxide, eg, water and sodium hydroxide (or other alkali metal hydroxide). May occur through interaction. In addition to the polycarboxylic acid polymer, the combination of sodium hydroxide and a second alkali source (eg, sodium metasilicate) serves to control the kinetics and thermodynamics of the coagulation process, and additional functional materials It is contemplated to provide a coagulation matrix that can be combined to form a functional solid composition. For example, polycarboxylic acid polymers and other functional components can have the effect of stabilizing hydroxide by acting as free water donors and / or acceptors.

  In other aspects of the invention, there may be aspects of ash hydration, such as coagulation as a result of the interaction of water with a hydratable salt. For example, according to such embodiments, the carbonate hydrates by acting as a free water donor and / or acceptor.

  According to aspects of the present invention, the solidification rate of the detergent composition is controlled by controlling the rate of water transfer relative to the hydration of the alkaline source of ash and / or hydroxide, and the resulting solid detergent composition product Can provide processing and dimensional stability. If the solidification matrix solidifies too quickly, the solidification rate is important because the composition may solidify during the mixing and stopping process. If the solidification matrix solidifies too slowly, valuable processing time is lost.

  Without being limited to a particular theory of the present invention, in one aspect, the polycarboxylic acid polymer ensures that a solid product comprising sodium hydroxide and a second alkali source (eg, sodium metasilicate) does not swell. This can help provide dimensional stability to the final product. Various problems arise when a solid product expands after solidification, including but not limited to reduced density, integrity, and appearance; and the lack of ability to dispense or package the solid product. In general, a solid product is considered dimensionally stable when it has an increase index of less than about 3%, particularly less than about 2%. The increase index intends the rate of product increase or swelling over a period of time after solidification under normal transport / storage conditions. Since normal shipping / storage conditions for detergent products often result in detergent compositions that are exposed to high temperatures, the increase index of a solid detergent product is one of the products before and after heating at 100 ° F. to 120 ° F. It can be determined by measuring more dimensions. The measured dimension or dimensions depend on the shape of the solid product and how it swells. For tablets, changes in both diameter and height are generally measured and added together to determine the growth index. For capsules, simply the diameter is usually measured.

  In general, a solid detergent composition using the coagulation matrix of the present invention comprises an alkali metal hydroxide alkali source (eg, sodium hydroxide), a second alkali source (eg, anhydrous sodium metasilicate), a polycarboxylic acid polymer, It can be created by combining sodium carbonate, water and additional functional ingredients, and allowing the ingredients to interact and coagulate.

  For example, in a first embodiment, the solid detergent composition may comprise sodium hydroxide, anhydrous sodium metasilicate, polycarboxylic acid polymer, water charge, sodium carbonate, chelating agent, and optional functional ingredients. it can. In an exemplary embodiment, the solid detergent composition comprises about 1% to 90% by weight alkali metal hydroxide alkali, about 0.1% to about 15% polycarboxylic acid polymer, about 0% 0.1 wt% to about 25 wt% water, about 20 wt% to about 90 wt% sodium carbonate, about 0.1 wt% to about 50 wt% sodium gluconate chelating agent, and about 0.1 wt% % By weight to about 50% by weight of a second alkali source and / or corrosion inhibitor. In another exemplary embodiment, the solid detergent composition has an alkalinity of about 5% to 70% by weight alkali metal hydroxide, 1% to about 10% polycarboxylic acid polymer, about 0.00%. 1 wt% to about 10 wt% water, about 25 wt% to about 90 wt% sodium carbonate, about 1 wt% to about 50 wt% chelating agent, and 1 wt% to 50 wt% second alkali source And / or contain a corrosion inhibitor. In yet another exemplary embodiment, the solid detergent composition comprises about 10% to 50% by weight alkali metal hydroxide alkali, 2.5% to about 10% polycarboxylic acid polymer, About 1% to about 5% water, about 30% to about 70% sodium carbonate, about 1% to about 50% chelating agent, and 1% to 50% secondary alkali Source and / or corrosion inhibitor. Without being limited to the scope of the invention, all numerical ranges set forth herein include values that define the range and include each integer within the specified range.

  In some embodiments, the relative amounts of sodium hydroxide, water and polycarboxylic acid polymer are controlled within the composition. The solidification matrix and the additional functional components harden to a solid form due to the chemical reaction of sodium hydroxide and water (hydroxide hydration) and / or water and sodium carbonate (ash hydration). As the solidification matrix solidifies, the binder composition can take shape to bind and solidify the components. At the same time the remainder of the components form the remainder of the solid composition, at least some of the components associate to form a binder. The solidification process may last from a few minutes to about 6 hours, depending on factors including, but not limited to, the size of the composition being formed, the components of the composition, and the temperature of the composition.

  According to one aspect of the invention, the hydratable salt (eg, sodium carbonate), the second alkali source (eg, anhydrous sodium metasilicate) and the at least one additional functional ingredient are in a homogeneous powder mixture. Mixed together. The source of water can be added to the homogeneous powder mixture prior to incorporation into the detergent composition and provided as a solid hydrate. According to one aspect of the invention, the addition of water to a homogeneous powder mixture is referred to herein as water “charge”. A water charge is included in the coagulation matrix for subsequent combination with sodium hydroxide (and optionally a polycarboxylic acid polymer). In one aspect, the water charge is preferably less than about 10%, from about 1% to about 10%, or from about 2% to about 10%.

  The solid hydrate is then combined with sodium hydroxide (and optionally a polycarboxylic acid polymer). When added to a detergent composition, sodium hydroxide is combined with a water and sodium carbonate matrix to effectively coagulate the detergent composition according to the method of the present invention. In general, the effective amount of sodium hydroxide and sodium carbonate is controlled by controlling the rate and movement of water into the hydroxide hydration process and / or ash hydration process, and A quantity that effectively controls thermodynamics is intended.

  Solid detergent compositions formed using a coagulation matrix are produced using a batch or continuous mixing system. In an exemplary embodiment, the tablet press processing method is used to form tablets from a homogeneous mixture in accordance with the method of the present invention. In some embodiments, the processing temperature is the melting temperature of the component or less. The processed mixture can be molded or dispensed from the mixer by other suitable means so that the detergent composition cures to a solid form. The structure of the matrix can be characterized by its hardness, melting point, material distribution, crystal structure, and other similar properties by methods known in the art. In general, a solid detergent composition treated according to the method of the present invention is substantially homogeneous and dimensionally stable with respect to the distribution of components throughout its mass.

  Specifically, in the molding process, liquid and solid components are introduced into the final mixing system and the components produce a substantially homogeneous semi-solid mixture, which components are dispersed throughout the mass. Until continuously mixed. In an exemplary embodiment, the components are mixed in a mixing system for at least about 5 seconds. The mixture is then discharged from the mixing system into or through a die or other forming means. The product is then packaged. In an exemplary embodiment, the formed composition begins to cure to a solid form in less than 1 minute, or from about 1 minute to about 3 hours. In particular, the formed composition begins to cure to a solid form within a few seconds to about 1 minute. More specifically, the formed composition begins to harden to a solid form within a few seconds to about 2 minutes.

  With respect to the term “solid form”, it is meant that the cured composition does not flow and will substantially retain its shape under moderate stress or pressure or simply gravity. The hardness of the solid composition can range from a relatively dense and hard fused solid product, such as concrete, to a consistency characterized as a hardened paste. Furthermore, the term “solid” intends the state of the detergent composition under the expected conditions of storage and use of the solid detergent composition. In general, it is expected that the detergent composition will remain in solid form when exposed to temperatures up to about 100 ° F. and in particular above about 120 ° F.

  The resulting solid detergent composition can take forms including but not limited to extruded, molded or molded solid pellets, blocks, tablets, powders, granules, flakes; The resulting solid can then be ground or formed into powders, granules or flakes. In an embodiment of the invention, the solid detergent composition is not a cast solid product. In an exemplary embodiment, the extruded pellet material formed by the solidified matrix has a weight of about 50 grams to about 250 grams, and the extruded solid formed by the solidified matrix is about 100 grams or more. And a solid block detergent formed by the coagulation matrix, having a mass of about 0.25 to about 10 kilograms. The solid composition provides a stabilized source of functional material. In some embodiments, the solid composition can be dissolved, for example, in an aqueous medium or other medium to make a concentrated and / or use solution. The solution may be directed to a storage container for later use and / or dilution, or applied directly to the place of use.

  In certain embodiments, the solid detergent composition is provided in unit dosage form. A unit dose means a solid detergent composition unit sized so that all units are used during a single wash cycle. According to aspects of the present invention, when the solid detergent composition is provided as a unit dose, it is typically provided as an extruded pellet or tablet having a size of from about 1 gram to about 250 grams.

  In other embodiments, the solid detergent composition is provided in the form of a variety of use solids, such as blocks or a plurality of pellets, and is used repeatedly to produce an aqueous detergent composition for a variety of wash cycles. Can be done. In certain embodiments, the solid detergent composition is provided as an extruded block or tablet having a mass of about 5 grams to about 10 kilograms. In certain embodiments, various use forms of the solid detergent composition have a mass of about 1 kilogram to about 10 kilograms. In a further embodiment, the various use forms of the solid detergent composition have a mass of about 5 kilograms to about 8 kilograms. In other embodiments, the various use forms of the solid detergent composition have a mass of from about 5 grams to about 1 kilogram, or from about 5 grams to about 500 grams.

  Although the detergent composition is described as being formed into a solid product, the detergent composition can also be provided in the form of a paste. If the concentrate is provided in the form of a paste, sufficient water is added to the detergent composition so that complete solidification of the detergent composition is eliminated. Dispersants and other ingredients may also be incorporated into the detergent composition to maintain the desired distribution of ingredients.

  The various coagulation matrices of the present invention can be used for a wide variety of cleaning applications. In some embodiments, the solid detergent compositions of the present invention are suitable for use in applications that require environmentally friendly, solid alkaline detergents. Such applications include, but are not limited to, the use of phosphate-free alkaline detergents in combination ovens, such as those used in various food service industries. Further applications include, for example, dishwashers employing dishwashing detergents, detersive detergents, fly-ar boilouts, power soak sinks and related applications, soak tanks, rework of utensils, laundry and fabric washing and decontamination , Carpet cleaning and decontamination, vehicle cleaning and care applications, surface cleaning and decontamination, kitchen and bath cleaning and decontamination, floor cleaning and decontamination, cleaning work in place, general purpose It may include cleaning and destaining and / or industrial or household cleaning agents.

  In a preferred embodiment, the solid detergent composition is particularly suitable for cleaning a combination oven. Various descriptions of combination ovens are described in US Pat. No. 5,368,008, US Pat. No. 5,640,946, and US Pat. No. 6,410,890, published European patent application. No. 0652405 and German Patent Application No. 2842771, each of which is incorporated herein by reference in its entirety. For example, a combination oven may contemplate an appliance having a double oven steamer, a double oven boiler, or having at least one oven chamber and a steam generator and / or boiler. The solid detergent composition of the present invention may be provided for cleaning combination oven appliances known in the art.

  In some embodiments, instead of having to access the combination oven steamer and / or boiler components, for example, as described and depicted in US Pat. No. 5,640,946. The solid detergent composition can be added directly to the combination oven apparatus via a funnel or other member. These and other injection points for supplying a solid detergent composition according to the present invention will be readily ascertainable by one skilled in the art. In some embodiments, the solid detergent composition according to the present invention can be used initially to produce an aqueous solution or suspension for delivery to a combination oven for cleaning according to the present invention. The liquid composition is then applied to the internal surface of the device, such as by use of a spray nozzle and / or spray jet.

  The cleaning method using the solid detergent composition of the present invention may further include one or more rinsing steps, decalcification steps, pre-cleaning steps, and / or dipping steps.

  Since many modifications and variations within the scope of the invention will be apparent to those skilled in the art, the invention will be more specifically described in the following examples, which are intended to be exemplary only. Unless otherwise noted, all parts, percentages, and ratios reported in the following examples are by weight, and all reagents used in the examples are obtained from the following chemical suppliers: Alternatively, it can be obtained or synthesized by conventional techniques.

  The following test methods were used to characterize the compositions prepared in Examples 1, 2, and 3 and Comparative Examples A and B.

Mold Dimensional Stability Test About 50 grams of a batch of product using polycarboxylic acid polymer as part of the solidification matrix was first pressed in a die at about 1000 pounds per square inch (psi) for about 20 seconds. Formed a tablet. The tablet diameter and height were measured and recorded. The tablets were kept at room temperature for 1 day and then placed in an oven at a temperature of about 120 ° F. After removing the tablet from the oven, the tablet diameter and height were measured again and recorded. The growth index was determined for the tablets by measuring the increase based on cumulative changes in tablet diameter and height after heating.

Examples 1, 2, and 3 and Comparative Examples A and B
Examples 1, 2, and 3 are compositions of the present invention using a polycarboxylic acid polymer as part of the coagulation matrix. In particular, the compositions of Examples 1, 2, and 3 used a polyacrylic acid polymer, a modified polyacrylic acid polymer, and a polymaleic acid polymer, respectively, as part of the coagulation matrix. In addition, the compositions of Examples 1, 2, and 3 also provided sodium carbonate (soda ash or heavy ash), sodium bicarbonate, sodium metasilicate, builder, surfactant, Ingredient concentrations (weight percent) of foaming agent, sodium hydroxide and water were included. Sodium carbonate, sodium bicarbonate, sodium metasilicate, builder, surfactant, and antifoam are premixed to form a powder premix, and polycarboxylic acid polymer, sodium hydroxide and water are premixed to form a liquid A premix was formed. The powder premix and liquid premix were then mixed together to form a composition. About 50 grams of the composition was pressed into a tablet at about 1000 psi for about 20 seconds.

  The composition of Comparative Example A was prepared as in Examples 1, 2, and 3, except that the composition of Comparative Example A did not contain a polycarboxylic acid polymer.

  A composition of Comparative Example B was prepared as in Example 1 except for the addition of Trilon M powder, which was methyl glycine diacetate (MGDA) powder. Table 1 provides component concentrations for the compositions of Examples 1, 2, and 3 and Comparative Example A. Table 2 provides the component concentrations of Comparative Example B.

  Subsequently, in order to observe the dimensional stability of the composition after heating, as described above, the compositions of Examples 1, 2, and 3 and Comparative Example A were subjected to a dimensional stability test on the molded article. . The results are shown in Table 3 below.

  As shown in Table 3, the molded articles of the compositions of Examples 1, 2, and 3 showed significantly less swelling than the molded articles of the composition of Comparative Example A. In particular, the product of the composition of Example 1 had only a 0.6% increase in diameter and a 1.1% increase in height, resulting in an increase index of 1.7%. The product of the composition of Example 2 had a 0% increase in diameter and a -0.6% increase in height and did not provide a positive increase index. The product of the composition of Example 3 had only a 0.9% increase in diameter and a 1.2% increase in height, resulting in an increase index of 2.1%. In comparison, the product of the composition of Comparative Example A had a 2.7% increase in diameter and an 8.2% increase in height, resulting in an increase index of 10.9%.

  The only difference in the compositions of Examples 1, 2, and 3 and Comparative Example A was the presence of polycarboxylic acid polymer. Thus, the polycarboxylic acid polymer is believed to have helped the dimensional stability of the products of the compositions of Example 1, Example 2, and Example 3. Since the composition of Comparative Example A did not contain a polycarboxylic acid polymer, the composition did not include a mechanism for controlling the movement of water within the solid product.

  Six tablet samples of the composition of Comparative Example B were also subjected to a swelling test. The diameter and height of each such tablet was measured and recorded. The tablets were maintained at room temperature for 1 day and then placed in an oven heated to a temperature of about 120 ° F. When the first tablet was removed from the oven, the tablet shattered, indicating a lack of dimensionally stable product. The remaining samples were successfully removed from the oven and the diameter and height of each tablet was measured and recorded as described in Table 4 below.

  As can be seen by the results in Table 4, each of samples 1, 2, 3, 4, 5 and 6 containing MGDA is not stable and / or 4.5% when exposed to 120 degrees Fahrenheit. Increased over.

Dimensional stability test for cast products A batch of about 4000 grams of product using polycarboxylic acid polymer as part of the coagulation matrix was first poured into capsules. The diameter of the capsule was measured and recorded. The capsules were maintained at room temperature for 1 day and kept in an oven at a temperature of about 104 ° F. for 2 days before returning to room temperature. After returning the capsules to room temperature, the capsule diameter was again measured and recorded. The increase index was determined for the capsules by measuring the increase based on the change in diameter after heating.

Examples 4, 5, and 6 and Comparative Example C
Examples 4, 5, and 6 are compositions of the present invention that use a polycarboxylic acid polymer as part of the coagulation matrix. In particular, the composition of Example 4 uses a polyacrylic acid polymer as part of the coagulation matrix, and the composition of Example 5 uses a modified polyacrylic acid polymer as part of the coagulation matrix. The composition used polymaleic acid polymer as part of the coagulation matrix. Each of Examples 4, 5, and 6 is also soft water, builder, water conditioner, sodium hydroxide 50%, sodium carbonate (heavy ash), anionic surfactant, and as provided in Table 3. Contains component concentrations (in weight percent) of nonionic surfactants. The liquid (soft water, builder, water conditioner, polycarboxylic acid polymer, and sodium hydroxide 50%) is premixed to form a liquid premix and the powder (sodium carbonate, anionic surfactant) , And nonionic surfactant) were premixed to form a powder premix. The liquid premix and powder premix were then mixed to form a composition, which was subsequently poured into capsules.

  The composition of Comparative Example C does not contain a polycarboxylic acid polymer but is prepared as in Examples 4, 5, and 6 except that it contains the same amount of available water. did.

  Table 5 provides component concentrations for the compositions of Examples 4-6 and Comparative Example C.

  After forming Examples 4, 5, and 6 and Comparative Example C, they were subjected to dimensional stability testing on cast products as described above to observe the dimensional stability of the composition after heating. . The results are shown in Table 6 below.

  As shown in Table 4, the cast products of the compositions of Examples 4, 5, and 6 showed significantly less swelling than the cast product of the composition of Comparative Example C. In particular, the product of the composition of Example 4 experienced only a 0.6% increase in diameter, resulting in an increase index of 0.6%, and the product of Example 5 increased only 1.3% in diameter. Experienced resulted in an increase index of 1.3%, and the product of the composition of Example 6 experienced only a 1.9% increase in diameter, resulting in an increase index of 1.9%. In comparison, the product of the composition of Comparative Example C has a 4.9% increase in diameter, resulting in an increase index of 4.9%.

  The only difference in the compositions of Examples 4, 5, and 6 and Comparative Example C was the presence of polycarboxylic acid polymer. Thus, the polycarboxylic acid polymer is believed to have helped the dimensional stability of the products of the compositions of Examples 4, 5, and 6. In contrast, since the composition of Comparative Example C did not contain a polycarboxylic acid polymer, the composition did not include a mechanism for controlling water movement within the solid product.

Examples 7, 8 and 9
Examples 7, 8 and 9 compare cleaning performance when various combinations of polymaleic acid and polyacrylic acid were utilized. The composition of each example is listed in Table 7. Premix sodium carbonate, builder, surfactant, and disaccharide to form a composition, form a powder premix, and premix polycarboxylic acid polymer, potassium hydroxide, phosphonate and water to form the composition And a liquid premix was formed. The powder premix and liquid premix were then mixed together to form a composition. About 1000 grams of the composition was pressed into a tablet at about 1000 psi for about 20 seconds to solidify.

  The resulting tablet was employed in an AM-14 automatic dishwasher that dispenses 17 grains of water. The glassware was then subjected to 100 washing and rinsing cycles and tested for cleanliness. Cleanliness was measured in two ways. First, the brightness value was determined by taking a digital optical image of the glassware and then analyzing the brightness value by computer analysis. The brightness test indicates the degree of film present on the glass surface, with lower values indicating less film and cleaner glass. Second, the visual rating is measured on a scale of 1-5, with a lower visual rating indicating a cleaner glass. The results of these tests are listed in Table 8.

  The results listed in Table 8 indicate that the combination of polymaleic acid and polyacrylic acid provides improved cleaning performance over polymaleic acid or polyacrylic acid alone.

Examples 10-23
Employing a series of experiments using different concentrations and sources of water, chelating agent, and binder to evaluate the use of sodium hydroxide alkalinity to produce a solid alkaline detergent composition in accordance with the objectives of the present invention. did. In order to provide a method of making a physically stable and durable cleaning composition according to the present invention, various formulations and mixing instructions (mixes) for making solid, phosphate-free alkaline detergent tablets instructions). Table 9 shows the components evaluated, potassium carbonate (alkali builder); sodium sulfate (filler); sodium gluconate (chelating agent); disodium metasilicate (alkali source, corrosion inhibitor); sodium hydroxide (active) Detergent, caustic); and PEG (binder).

  Good batch mixing and powder movement were observed for Examples 10-23. The appearance of the powder varied from batch to batch and the particle size uniformity was dependent on the content of polyethylene glycol (PEG). Visual evaluation showed that the powder without PEG in the composition was most uniform, but aggregate formation increased as the amount of PEG in the formulation increased. Agglomerates form when molten PEG is added to the batch during mixing.

Dimensional stability test for extruded and pressed solids Screened at 2500, 3000, and 4000 pounds. We found that a press at 4000 pounds produced the best tablet. Tablets made with this load had good sharp edges, smooth surfaces and high compressive strength. Tablets made with the other two loads had a more porous surface and weak edges. The tablet release from the press mold for all 14 runs was inadequate. After every 2-3 pressed tablets, it was necessary to wash the press head until there was no residue. For example, if the residue is not removed after the third tablet, then the fourth tablet will not leave the press head and will be removed either by blunting or dissolving the tablet with water Would be only.

  Using PEG 8000 as a potential binder in high alkali formulations browned the tablet over time. Color stability was dependent on how much PEG was included in the formulation. Examples 12 and 19 did not contain PEG and showed no discoloration over time. For all examples that contained PEG 8000, brown color was observed as early as 1 day in a 122 ° F. chamber.

Dimensional stability Initial height, diameter, and appearance were recorded. The tablets were then sealed in plastic bags and placed in two different environmental chambers for a week. The two environmental chambers used were an atmosphere (72 ° F., 50% relative humidity) and 122 ° F. (relative humidity NA). One week later, the tablet was measured again and the appearance was recorded.

Procedure for Determining the Compression Resistance of Extruded and Pressed Products One tablet from each batch was tested within 3 hours of being made. After the weekly dimensional stability test was completed, the 122 ° F. tablets were cooled to ambient conditions and then the compressive strength was measured for both sets of tablets. The tested formulations were not physically stable at 122 ° F. Tablets swelled 4% to 10% and tablets containing both PEG 8000 and sodium hydroxide turned brown. The results show that the composition according to the invention does not contain PEG as a preferred binder for a stable, phosphate-free alkaline oven cleaner tablet composition.

Examples 24-29
Based on the results of Examples 10-23, an alternative coagulation mechanism, namely carbonate hydration, was further evaluated. Potassium hydroxide and sodium carbonate were evaluated to determine their effect on the stability of tablets with different chelating agents.

  Table 10 shows the components evaluated, potassium carbonate / potassium (alkali builder); sodium carbonate / ash (alkali builder); sodium citrate (chelating agent, binder); sodium hydroxide (active detergent, caustic, water) (50%)); water (hydration); disodium metasilicate (alkali source, corrosion inhibitor); and sodium sulfate (filler).

  Potassium carbonate, sodium carbonate and sodium citrate were added to the ribbon blender and mixed. Sodium hydroxide (50%) and water were added and mixed until the powder appeared dry. Disodium metasilicate, sodium sulfate and sodium hydroxide were added and mixed until the powder appeared uniform. Examples 24-29 did not provide adequate mixing (the powder was moist, agglomerated, and difficult to remove from the ribbon blender). Due to insufficient mixing, the powder was not pressed into tablets and the experiment was terminated.

Examples 30-38
Based on the results of Examples 24-29, the use of sodium carbonate instead of potassium carbonate was evaluated. In order to obtain a more physically stable tablet formulation, the use of sodium carbonate (heavy ash) was evaluated in the composition.

  Table 11 shows the components evaluated, sodium carbonate (alkali builder); sodium citrate (chelating agent, binder); citrate solution (33%); sodium hydroxide (active detergent, caustic, hydration (50 %)); Water (hydration); disodium metasilicate (alkali source, corrosion inhibitor); and sodium sulfate (filler).

  For Examples 30-36, sodium carbonate was added to the ribbon blender and mixed. Sodium citrate was added slowly. The water / citrate solution and disodium metasilicate were then mixed until the powder was uniform. The 60 gram tablet was then held for 3 seconds using a 1.75 "diameter tablet die and Carver press and pressed at 4000 lbs (about 1600 psi) and 2500 lbs. Then needed to break the tablet (The higher force / pressure required translates into a more durable tablet.) The tablets were then placed in a one week dimensional stability test at room temperature and 122 ° F.

  For Examples 37-38, sodium carbonate and sodium citrate were added to the ribbon blender and mixed. Water and disodium metasilicate were added and mixed until the powder was uniform. The 60 gram tablet was then held for 3 seconds using a 1.75 "diameter tablet die and a Carver press and pressed at 4000 lbs (about 1600 psi) and 2500 lbs. Force required to break the tablet (The higher force / pressure required translates into a more durable tablet.) The tablets were then placed in a one week dimensional stability test at room temperature and 122 ° F.

  The tested formulation was physically stable at 72 ° F, while the formulation was not physically stable at 122 ° F. The tablets swelled 9% -18% and the compressive strength was weak in all Examples 30-38. Example 33 showed improved compressive strength and dimensional stability compared to the other examples, but the formulation required further improvements to coagulation and dimensional stability.

Examples 39-42
Based on the results of Examples 30-38, the use of different grades of sodium metasilicate was evaluated. To evaluate the improvement of coagulation and dimensional stability, anhydrous sodium metasilicate was used in formulations with potassium carbonate at lower water levels. Table 12 shows the ingredients evaluated in the compositions of the examples.

  For Examples 39-40, potassium carbonate and sodium citrate were added to the ribbon blender and mixed. Water was added slowly. The disodium metasilicate, sodium sulfate and sodium hydroxide were then mixed until the powder was uniform. The 25 gram tablet was then held for 3 seconds using a 1.25 "diameter tablet die and a Carver press and pressed at 2000 pounds. The force required to break the tablet was then measured (required) (A higher force / pressure translates into a more durable tablet.) The tablets were then placed in a one week dimensional stability test at room temperature and 122 ° F.

  For Examples 41-42, sodium carbonate, sodium citrate and anhydrous metasilicate were added to the ribbon blender and mixed. Water was added slowly. The sodium hydroxide was then mixed until the powder was uniform. The 25 gram tablet was then held for 3 seconds using a 1.25 "diameter tablet die and a Carver press and pressed at 2000 pounds. The force required to break the tablet was then measured (required) (A higher force / pressure translates into a more durable tablet.) The tablets were then placed in a one week dimensional stability test at room temperature and 122 ° F.

  As shown in FIGS. 1-2, the formulation of the tablet composition with anhydrous sodium metasilicate produced stronger tablets with less swelling than the conventional example using disodium metasilicate pentahydrate. The examples also show that the use of potassium carbonate can yield a dimensionally stable solid composition when the water charge used during mixing is less than about 1%. . However, the additional advantage of using sodium carbonate, i.e. improved cleaning performance, provides its preferred use over potassium carbonate.

Examples 43-46
Based on the results of Examples 39-42, the use of various concentrations and sources of water was evaluated to make a durable and physically stable tablet composition. Table 13 shows the components evaluated in the compositions of the examples.

  For Examples 43-46, sodium carbonate, d-gluconic acid, sodium citrate, sodium metasilicate and / or anhydrous metasilicate were added to the ribbon blender and mixed. Water was added slowly. The sodium polyacrylate polymer and sodium hydroxide were then mixed until the powder was uniform. The 60 gram tablet was then held for 3 seconds using a 1.75 "diameter tablet die and Carver press and pressed at 4000 lbs (about 1600 psi) and 2500 lbs. Then needed to break the tablet (The higher force / pressure required translates into a more durable tablet.) The tablets were then placed in a one week dimensional stability test at room temperature and 122 ° F.

  As shown in FIGS. 3-4, the example formulation mixed with the liquid water charge had higher compressive strength than the example formulation without the free water charge. Example 45 yielded the hardest tablet with the least amount of swelling (showing maximum dimensional stability).

  Although the present invention has been described with reference to preferred embodiments, those skilled in the art will recognize that modifications can be made in form and detail without departing from the spirit and scope of the invention.

  Various changes and additions can be made to the discussed exemplary embodiments without departing from the scope of the present invention. For example, while the above-described embodiments refer to particular features, the scope of the present invention also includes embodiments having different combinations of features and embodiments that do not include all of the features described above.

All publications and patent applications in this specification are indicative of the level of ordinary skill in the art to which this invention pertains. All publications and patent applications are hereby incorporated by reference to the same extent as if each individual publication or patent application was specifically and individually indicated by reference. A part of the embodiment of the present invention is described in the following items [1] to [20].
[Item 1]
An alkali source of alkali metal hydroxide;
Sodium carbonate,
A second alkali source of anhydrous silicate,
water and,
A solid detergent composition comprising at least one functional ingredient,
When the solid detergent composition is phosphorus free and heated at a temperature of 120 degrees Fahrenheit, the solid detergent composition is a dimensionally stable hydrated solid having an increase index of less than 3%. A solid detergent composition.
[Item 2]
Item 2. The item 1, wherein the at least one functional component is selected from the group consisting of a second alkali source, a detergent builder, a surfactant, a corrosion inhibitor, a water conditioner, a chelating agent, a flow aid, and combinations thereof. Composition.
[Item 3]
Item 2. The composition according to Item 1, wherein the functional component is a polyacrylic acid polymer or a salt or derivative thereof.
[Item 4]
Item 2. The composition according to Item 1, wherein the functional component is a polycarboxylic acid polymer that is a polyacrylic acid polymer or a polyacrylate polymer, and constitutes about 0.1 wt% to about 15 wt% of the composition.
[Item 5]
The composition of item 1, wherein the sodium carbonate comprises from about 20% to about 90% by weight of the composition.
[Item 6]
The composition of item 1, wherein water comprises from about 0.1% to about 10% by weight of the composition.
[Item 7]
The composition according to item 1, wherein the composition does not comprise one or more polyethylene glycols and / or urea.
[Item 8]
Item 2. The composition according to Item 1, wherein the alkali metal hydroxide is sodium hydroxide and constitutes about 5% to 70% by weight of the composition.
[Item 9]
The composition according to item 1, wherein the at least one functional ingredient is a second alkali source and constitutes about 1% to 50% by weight of the composition.
[Item 10]
The composition according to item 1, wherein the at least one functional ingredient is a chelating agent and constitutes about 1% to 50% by weight of the composition.
[Item 11]
2. The composition of item 1, wherein the composition is a hydrated solid tablet.
[Item 12]
About 5% to about 70% by weight of sodium hydroxide of the solid detergent composition;
About 20% to about 90% by weight of sodium carbonate of the solid detergent composition;
From about 0.1% to about 15% by weight of the solid detergent composition of a polycarboxylic acid polymer or salt or derivative thereof;
About 0.1% to about 10% water by weight of the solid detergent composition;
A second alkali source of about 1% to about 50% by weight of a second detergent source, wherein the alkali source is anhydrous metasilicate;
A solid detergent composition consisting essentially of from about 1% to about 50% by weight of a chelating agent of the solid detergent composition, wherein the solid detergent composition is a hydrate solid that does not contain phosphorus The solid detergent composition is dimensionally stable when heated at a temperature of 120 degrees Fahrenheit and has an increase index of less than 3%.
[Item 13]
Sodium hydroxide comprises about 10% to 50% by weight of the composition, sodium carbonate comprises about 30% to 70% by weight of the composition, and the polycarboxylic acid polymer or salt or derivative thereof is a polyacrylate polymer About 2.5% to 10% by weight of the composition, water constitutes about 1% to 5% by weight of the composition, and the second alkali source is about 1% to about 5% by weight of the composition. 13. A composition according to item 12, comprising 20% by weight and the chelating agent comprising about 5% to 25% by weight of the composition.
[Item 14]
14. A composition according to item 13, wherein the composition is a hydrated solid tablet without one or more polyethylene glycols, urea and / or potassium carbonate.
[Item 15]
A method of forming a solid detergent composition comprising:
Combining sodium carbonate, a second alkali source of silicic acid anhydride and at least one additional functional ingredient to form a powder premix;
Mixing the powder premix with a water source to form a solid hydrate;
Mixing the solid hydrate with a source of sodium hydroxide and optionally a polycarboxylic acid polymer or salt or derivative thereof,
When the solid detergent composition is phosphorus free and heated at a temperature of 120 degrees Fahrenheit, the solid detergent composition is dimensionally stable and has an increase index of less than 3% Forming method.
[Item 16]
Item 16. The method according to Item 15, wherein the solid detergent composition is a tablet.
[Item 17]
The solid detergent composition comprises, among the solid detergent compositions, about 5% to about 70% by weight of sodium hydroxide, about 20% to about 90% by weight of sodium carbonate, a polycarboxylic acid polymer or a salt or derivative thereof. 0.1 wt% to about 15 wt%, water about 0.1 wt% to 10 wt%, secondary alkali source about 1 wt% to about 50 wt%, and chelating agent about 1 wt% to about 50 wt% Item 16. The method according to Item 15, comprising mass%.
[Item 18]
16. The method of item 15, further comprising solidifying the composition at an ambient temperature of about 30 ° C to about 50 ° C.
[Item 19]
16. A method according to item 15, wherein the dimensional stability of the solid detergent composition has an increase index of less than 2%.
[Item 20]
Sodium hydroxide comprises about 10% to 50% by weight of the composition, sodium carbonate comprises about 30% to 70% by weight of the composition, and the polycarboxylic acid polymer or salt or derivative thereof is a polyacrylate polymer Or a salt or derivative thereof, comprising about 2.5% to 10% by weight of the composition, water comprising about 1% to 5% by weight of the composition, and the second alkali source being the composition. 16. The method of item 15, comprising about 1% to 20% by weight and the chelating agent comprising about 5% to 25% by weight of the composition.

Claims (18)

5% to 70% by weight of an alkali metal hydroxide of the solid detergent composition;
20% to 90% by weight of sodium carbonate or potassium carbonate of the solid detergent composition;
1% to 50% by weight of anhydrous metasilicate of the solid detergent composition;
0.1 wt% to 10 wt% water of the solid detergent composition;
A solid detergent composition comprising from 1% to 50% by weight of the solid detergent composition of at least one functional ingredient,
The sodium carbonate or potassium carbonate, the anhydrous metasilicate and the at least one functional ingredient are mixed to form a powder premix, and then the powder premix is mixed with the water to form a solid hydrate A solid detergent composition formed by mixing the solid hydrate with the alkali metal hydroxide, the solid detergent composition being free of phosphorus and in the form of blocks, pellets, or tablets. A solid detergent composition that is dimensionally stable hydrate solid when heated at a temperature of 120 degrees Fahrenheit and has an increase index of less than 3%.   The composition of claim 1, wherein the at least one functional ingredient is selected from the group consisting of detergent builders, surfactants, corrosion inhibitors, water conditioners, chelating agents, flow aids, and combinations thereof.   The composition of claim 1, wherein the composition further comprises 0.1% to 15% by weight of the composition of a polyacrylic acid polymer or polyacrylate polymer.   The composition according to claim 1, wherein sodium carbonate or potassium carbonate constitutes 30% to 70% by weight of the composition.   The composition of claim 1, wherein the composition does not comprise one or more polyethylene glycols and / or urea.   The composition according to claim 1, wherein the alkali metal hydroxide is sodium hydroxide.   The composition of claim 1, wherein the anhydrous metasilicate comprises 10% to 35.5% by weight of the composition.   The composition of claim 1, wherein the at least one functional ingredient is a chelating agent.   The composition of claim 1, wherein the solid detergent composition is a hydrated solid tablet. 5% to 70% by weight sodium hydroxide of the solid detergent composition;
20% to 90% by weight sodium carbonate of the solid detergent composition;
0.1 wt% to 15 wt% of a polycarboxylic acid polymer or salt thereof in the solid detergent composition;
0.1 wt% to 10 wt% water of the solid detergent composition;
1% to 50% by weight of anhydrous metasilicate of the solid detergent composition;
1 mass% to 50 mass% of the chelating agent in the solid detergent composition, a solid detergent composition comprising,
The sodium carbonate, the anhydrous metasilicate and the chelating agent are combined to form a powder premix, then the powder premix is mixed with the water to form a solid hydrate, and then the solid water A solid detergent composition formed by mixing a hydrate with the sodium hydroxide and the polycarboxylic acid polymer or a salt thereof, the solid detergent composition being a hydrate solid containing no phosphorus, a block, A solid detergent composition that is in the form of pellets or tablets, is dimensionally stable when heated at a temperature of 120 degrees Fahrenheit, and has an increase index of less than 3%.   Sodium hydroxide constitutes 10% by mass to 50% by mass of the composition, sodium carbonate constitutes 30% by mass to 70% by mass of the composition, and the polycarboxylic acid polymer or a salt thereof is a polyacrylate polymer. 2.5% to 10% by weight of the product, water constitutes 1% to 5% by weight of the composition, anhydrous metasilicate constitutes 1% to 20% by weight of the composition, The composition according to claim 10, wherein the chelating agent comprises 5% to 25% by weight of the composition.   11. The composition of claim 10, wherein the solid detergent composition is a hydrated solid tablet without one or more polyethylene glycols, urea and / or potassium carbonate. A method of forming a solid detergent composition comprising:
20% to 90% by weight of the composition sodium carbonate or potassium carbonate, 5% to 50% by weight of the composition of anhydrous metasilicate and at least one additional function of 1% to 50% by weight of the composition Mixing the ingredients to form a powder premix;
Mixing the powder premix with 0.1% to 10% water by weight of the composition to form a solid hydrate;
Combining the solid hydrate with 10% to 50% sodium hydroxide by weight of the composition and optionally 0.1% to 15% by weight polycarboxylic acid polymer or salt thereof of the composition; With
When the solid detergent composition is phosphorus free, in the form of blocks, pellets, or tablets and is heated at a temperature of 120 degrees Fahrenheit , it is dimensionally stable and has an increase index of less than 3%. A method for forming a solid detergent composition.   14. The method of claim 13, wherein the solid detergent composition is a tablet.   The solid detergent composition according to claim 13, wherein the solid detergent composition comprises 0.1% by mass to 15% by mass of a polycarboxylic acid polymer or a salt thereof, and 1% by mass to 50% by mass of a chelating agent. Method.   The method of claim 13, further comprising solidifying the composition at an ambient temperature of 30 ° C. to 50 ° C.   14. The method of claim 13, wherein the dimensional stability of the solid detergent composition has an increase index of less than 2%.   Sodium hydroxide constitutes 10% by mass to 50% by mass of the composition, sodium carbonate constitutes 30% by mass to 70% by mass of the composition, and the polycarboxylic acid polymer or a salt thereof is a polyacrylate polymer or a fatty acid end group. A polyacrylic acid polymer or a salt thereof modified by the above, constituting 2.5 mass% to 10 mass% of the composition, water constituting 1 mass% to 5 mass% of the composition, 14. The method of claim 13, wherein the salt comprises 1% to 20% by weight of the composition and the chelating agent comprises 5% to 25% by weight of the composition.

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