US3417024A - Treated phosphates - Google Patents

Treated phosphates Download PDF

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US3417024A
US3417024A US625884A US62588467A US3417024A US 3417024 A US3417024 A US 3417024A US 625884 A US625884 A US 625884A US 62588467 A US62588467 A US 62588467A US 3417024 A US3417024 A US 3417024A
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detergent
tablet
water
tablets
caustic
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Goldwasser Seymore
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Lever Brothers Co
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Lever Brothers Co
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Priority to CH1670564A priority Critical patent/CH471891A/de
Priority to SE15744/64A priority patent/SE306982B/xx
Priority to DEU11325A priority patent/DE1296297B/de
Priority to GB52782/64A priority patent/GB1093420A/en
Priority to DK642564AA priority patent/DK116612B/da
Priority to FR439A priority patent/FR1420795A/fr
Priority to BE657846A priority patent/BE657846A/xx
Application filed by Lever Brothers Co filed Critical Lever Brothers Co
Priority to US625884A priority patent/US3417024A/en
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/02—Inorganic compounds
    • C11D7/04—Water-soluble compounds
    • C11D7/06—Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/0065—Solid detergents containing builders
    • C11D17/0073—Tablets

Definitions

  • This detergent tablet contains a synthetic organic nonionic detergent, a phosphate, 0.48% to 2.6% sodium hydroxide, potassium hydroxide or silicates as a source of Na O or K 0 for forming a solution in water with a concentration based on equivalents of Na O of at least 23.5% as NaOH and 2% to 11% water.
  • This invention relates to treated phosphates. More particularly, it is concerned with detergent tablets or briquettes containing the treated phosphates.
  • the detergent tablets contain two classes of essential components, namely nonionic detergent and phosphate, which are used in certain critical amounts and have a certain critical nature as set forth hereinafter.
  • the detergent briquettes contain from about 4% to about 13% by weight, and preferably from about to about 12% by weight, of one or more synthetic organic nonionic nonsoap detergents.
  • the nonionic detergents are a well-known class of low sudsing detergents and are produced by the condensation of several moles of a hydrophilic alkylene oxide, such as ethylene oxide or propylene oxide, with a hydrophobic base, such as an alkylated phenol, a fatty alcohol, a fatty amine, a fatty amide, or the hydrophobic base formed by the condensation of propylene oxide with propylene glycol.
  • the alkyl phenolalkylene oxide condensates are generally prepared by condensing one mole of an alkyl phenol having from about 9 to about carbon atoms in the alkyl radical with from about 8 to about moles of an alkylene oxide, such as ethylene oxide or propylene oxide.
  • condensation product of one mole of dodecyl phenol with an average of 10 moles of ethylene oxide sold commercially under the name Sterox DI the condensation product of 1 mole of nonyl phenol with an average of 9 moles of ethylene oxide sold commercially under the name .Igepal CO-630
  • the condensation product of 1 mole of nonyl phenol with an average of 10 moles of ethylene oxide sold commercially under the name Tergitol NPX the condensation product of 1 mole of nonyl phenol with an average of 20 moles of ethylene oxide sold commercially under the name Igepal CO-850.
  • nonionic detergents which are condensation products of a fatty alcohol with an alkylene oxide is the condensate of 1 mole of tridecyl alcohol with an average of 10 moles of ethylene oxide sold commercially under the name Sterox AJ-100.
  • Condensates of tall oil with alkylene oxides also form nonionic detergents. Typical of these is the condensate of 1 mole of tall oil with an average of 10 moles of ethylene oxide sold commercially under the name Sterox CD.
  • the polyoxyalkylene alk-anols are also nonionic detergents and are made by the condensation of an alkylene oxide with a hydrophobic base formed by the condensation of propylene oxide with propylene glycol.
  • These nonionic detergents which are described in US. Patent No. 2,674,619 and are sold under the name Pluronic, have the following empirical formula HO 2 4 a. 3 4 b 2 4 C
  • the hydrophobic base portion of this nonionic detergent, i.e., the (C H O) portion generally has a molecular weight from 801 to 2100.
  • the amount of ethylene oxide in these compounds is represented by the sum of a plus 0 which is an integer such that the molecule contains from 0 to 90% of ethylene oxide.
  • Pluronic L-60 b represents a molecular weight of 1501 to 1800 and a plus 0 is an integer such that the molecule contains 0-10% ethylene oxide.
  • Pluronic L-61 b represents a molecular weight of 1500-1800 and a plus 0 is an integer such that the molecule contains 10 to 20% ethylene oxide.
  • Pluronic L-64 b represents a molecular weight of 1501-1800 and a plus 0 is an integer such that the molecule contains 40-50% ethylene oxide.
  • Pluronic F-38 b represents a molecular weight of 801-1000 and a plus 0 is an integer such that the molecule contains 80-90% ethylene oxide.
  • Pluronic F-68 12 represents a molecular weight of 1501-1800 and a plus 0 is an integer such that the molecule contains 80-90% ethylene oxide.
  • Pluronic P- [1 represents a molecular weight of 1801- 2100 and a plus 0 is an integer such that the molecule contains 50-60% ethylene oxide.
  • Suitable nonionic detergents are the diethanolamides of long chain fatty acids, such as lauric diethanolamide.
  • the phosphate component of the detergent briquettes is present therein in an amount from about 20% to about 95% by weight, and preferably in an amount of about 60% by weight. This amount of phosphate substantially prevents bleeding or oiling out or separation from the tablets of any normally liquid or oily nonionic detergent present therein. The lower the level of normally liquid or oily nonionic detergent present, the less phosphate is needed to prevent bleeding.
  • the phosphate can be tetrapotassium pyrophosphate, or pentasodium or pentapotassium tripolyphosphate.
  • the tripolyphosphate as used can be completely anhydrous or the commercial anhydrous variety containing small amounts of water, either uncombined or in the form of small amounts of tripolyphosphate hexahydrate up to, for example, about 1%.
  • sodium tripolyphosphate When sodium tripolyphosphate is used, it may be Type II (wherein the tripolyphosphate content contains at least 95 Form II), or if rapid disintegration as Well as rapid solubility is desired, it must be a mixture of Form I and Form IIin which one form may vary from 10% to 90%, and the other from 90% to 10% respectively, in order for the resulting detergent tablets to have a high rate of disintegration, even in unagitated water, as well as rapid solubility in water.
  • Commercial Type I sodium tripolyphosphate containing about 20% Form I and Form II is suitable.
  • Detergent tablets prepared from completely anhydrous or commercial anhydrous Type II sodium tripolyphosphate have relatively slow disintegration rates but acceptable solubility rates.
  • Detergent tablets prepared by using a tripolyphosphate which is entirely in the hexahydrate form are unsatisfactory, because such tablets have a relatively poor rate of disintegration and solubilization.
  • a portion of the tetrapotassium pyrophosphate of pentasodium or pentapotassium tripolyphosphates can be substituted by other phosphates.
  • ing the surface of the tablets is critical, because the use of 0.5% or more by weight of water on the tablet surfaces causes the surface to swell and pull away from the body of the tablets and thereby form a very fragile shell. This shell is very easily cracked and flakes away from the tablet leaving a core of untreated tablet which generally lacks suflicient abrasion resistance. This does not lessen friability but rather increases it. Moreover, the use of 0.5% or more by weight of water in the surface moistening treatment may also cause unsightly protuberances to appear on the surface of the tablets.
  • the pellets are aged for a time up to 8 hours or longer after the moistening treatment to harden the surface of the pellets.
  • This aging can be performed at room temperature or higher, although the aging temperature should not be so high as to have a deleterious effect on any of the components in the tablet, such as any perfume which might be present therein.
  • the detergent tablets of the above Table A were tested for abrasion resistance by rubbing them with a plain woven cotton cloth for three minutes. After this abrasion treatment, the pellets showed no loss in weight and the surface of the pellets remained smooth.
  • the fracture strength of these tablets was at least 10 pounds and in some instances as high as 40 pounds after 24 hours aging.
  • the fracture strength of these tablets was determined by a test which consisted in standing a tablet on edge on a spring scale and then pressing a lever down on the tablets until they fractured.
  • the amount of bleeding, oiling-out or separation of any normally liquid nonionic detergent component from these detergent tablets was determined by placing the tablets on brown absorbent paper and observing any dampening of the paper. These tablets showed no bleeding when left in contact with the absorbent medium for 48 hours.
  • the interlacing undesirable crystals may eventually lock the internal structure of the tablet together, and the tablet will disintegrate slowly in Water. Therefore, an undesirable type of crystallization during the agglomerating and compressing steps adversely affects the initial strength of the tablet after compression, and it adversely affects subsequently the solubility of the tablets.
  • the aforementioned undesirable type of crystals are needle-like crystals.
  • the water in the hydrated phosphate in the tablet causes growth in the longitudinal direction only to form the needle-like crystals.
  • the undesirable needle-like crystals provided by the acid decomposition products of the phosphate are indicated schematically in FIGURE 1.
  • the crystals described herein are further defined in accordance with the procedure for determining the crystallization in sodium tripolyphosphate.
  • approximately 0.20 gram of sodium tripolyphosphate are placed on a 3" x 1" x 1 mm. microslide.
  • Five to eight drops of water from a stirring rod are added to the sodium tripolyphosphate granules on the microslide.
  • a 25 sq. mm. glass coverslide is placed immediately on top of the granules and it is tilted to one side in order to form a thin film of liquid and granules.
  • the slide is observed at 3 minute intervals for 12 minutes by using a microscope adjusted to magnifications with polarized light.
  • the crystal formation in the phosphate, per se is considered to be the same as the crystal formulation in a table containing a detergent, such as a nonionic detergent, and a phosphate, such as sodium tripolyphosphate.
  • a mixture comprising a detergent, a phosphate, 0.48% to 2.6% caustic and 2% to 11% water in order that there is a concentration of at least 23.5% caustic in water.
  • the mixture is agglomerated to form granules which are then screened.
  • the mixture is compressed subsequently into the shape of tablets.
  • the crystal growth therein takes place in all directions to form plate-like crystals. 'The presence of the plate-like crystals do not have an adverse effect upon the initial strength of the compressed tablets and upon the solubility of the tablets in water.
  • Plate-like crystals are also known [Industrial Microscopy, supra; Handbook of Chemical Microscopy, supra], and they define a certain type of crystal formation. The crystals is recognized in the art. The desirable plate-like crystals are illustrated schematically in FIGURE 2.
  • Tablets are one of the four basic forms of detergent compositions. They are formed by compressing granules, and they are characterized by their relatively fast dissolving and disintegrating properties. Therefore, the terminology tablets does not include the three other forms of detergent compositions, i.e., particulate compositions, such as powders, beads, flakes, chips and agglomerates; fluid compositions, such as liquids, and pastes; and bars or cakes formed by casting or extruding and characterized by their relatively slow dissolving and disintegrating properties.
  • particulate compositions such as powders, beads, flakes, chips and agglomerates
  • fluid compositions such as liquids, and pastes
  • bars or cakes formed by casting or extruding and characterized by their relatively slow dissolving and disintegrating properties.
  • caustic As stated heretofore, it is critical to use between 0.48% and 2.6% of caustic with a concentration of at least 23.5% in water contained in the detergent tablet. If less than 0.48% of caustic is employed or if the concentration is less than 23.5%, it will not prevent sufficiently the formation of the undesirable needle-like crystals and it will not permit or promote sufficiently the formation of the plate-like crystals. 1f more than 2.6%, e.g., 2.8% of caustic is employed, no crystallization will occur and the mixture, e.g., the agglomerated mixture, will be mushy.
  • the 0.48% to 2.6% caustic in the tablet is the weight of equivalent Na O based on the total weight of the tablet.
  • a phosphate is another essential ingredient in the detergent tablet of the invention.
  • the amount of phosphate is not critical; however, it is generally between about and about 95% by weight, preferably between 40% and 70%, based upon the total weight of the tablet.
  • a phosphate is pentasodium tripolyphosphate, pentapotassium tripolyphosphate and mixtures thereof.
  • a phosphate includes the substitution of other phosphates, such as an amount up to 50% of trisodium orthophosphate (Na PO an amount up to of tetrasodium pyrophosphate (Na P O an amount up to 20% of tetrapotassium pyrophosphate (K ,P O and an amount up to 30% of pentasodium tripolyphosphate hexahydrate, for a portion of the pentasodium tripolyphosphate and pentapotassium tripolyphosphate.
  • Na PO trisodium orthophosphate
  • Na P O an amount up to of tetrasodium pyrophosphate
  • K ,P O tetrapotassium pyrophosphate
  • sodium tripolyphosphate i.e., pentasodium tripolyphosphate
  • it is suitable to use Form I sodium tripolyphosphate alone, Form II sodium tripolyphosphate alone or a combination of Form 1 and Form II sodium tripolyphosphates.
  • This is one of the advantages of the present invention since it is not critical to have a certain amount of Form I and a certain amount of Form II when sodium tripolyphosphate is employed in a detergent tablet.
  • Form I and Form II sodium tripolyphosphates and their properties are well-known in the art (US. Pat. Nos. 3,056,652 and 2,897,155).
  • a detergent is a nonionic detergent, an anionic detergent or a mixture thereof.
  • the detergent generally comprises about 4% to about 13% by weight, preferably, 9% to 12%, based upon the total weight of the detergent tablet.
  • the nonionic detergent may be any of those known in the art including the ones specifically mentioned above for the Black and Gray tablet.
  • the Pluronic-type detergents disclosed in US. Pat. No. 2,425,845 are applicable.
  • anionic detergent alone or in combination with a nonionic detergent.
  • Any surface-active agent recognized in the art as being an anionic detergent is suitable herein. This includes, among others, the following anionic detergents: alkylaryl sulfonates in which the alkyl portion may be either branched or straight chain, the acyl isothionates, the acyl taurates, alkyl sulfates, the sulfated fatty alcohol ethylene-oxide condensates, alkyl taurines, hydroxy-alkyl taurines and the N (2 alkyl)- sulfoalkanamides.
  • the weight ratio of the phosphate to nonionic detergent is within the range of about 2:1 to about 20:1.
  • Another advantage of the present invention is that a suitable product may be formed even if the phosphate to detergent ratio is not within the aforementioned range.
  • the detergent tablets of this invention may have other components optionally include therein.
  • a tablet may have one or more inorganic builder salts, such as sulfates, carbonates and silicates of an alkali metal. About 0.25% to about 75% by weight, preferably 19% to about 30%, of the builder salt may be used in the tablet. If a silicate is employed, however, the amount of silicate may be limited since it may contribute equivalents of Na O. As stated heretofore, the total caustic in the detergent tablet must be between 0.48% and 2.6%.
  • Other optional components include a small amount, e.g., up to about 1%, of fluorescent dyes or optical brighteners; soil-suspending agents; perfumes; water-disprsible colorants; pigments or dyes; and mixtures thereof.
  • the procedures heretofore described in the Black and Gray process are applicable for the preparation of the instant detergent tablets.
  • the essential components and optional components are blended together until a uniform mixture is obtained.
  • the caustic is combined with an aqueous silicate solution and the solution with the caustic is sprayed into a rotating drum with powdered phosphate and detergent therein.
  • the agglomerated mixture therefrom is usually screened.
  • the mixture is then compressed into tablets with any desired shape, such as a cylindrical shape.
  • the compressed tablets may be treated subsequently by moistening the surface of the tablets with 0.1% to 0.4% by weight of water.
  • the chilling may be performed by exposing the tablets to substantially quiescent or moving cold air at a temperature not above about F. for at least 5 minutes.
  • a detergent tablet is provided from a detergent, a phosphate, water and a critical amount and concentration of caustic.
  • This tablet is substantially free from undesirable needle-like crystals as evidenced by its relatively high initial (fresh) strength after being compressed and by its ability to dissolve in water in less than about 1% minutes under the usual household washing machine operating conditions.
  • the tablet of the invention has the required plate-like crystals as evidenced by the fact that the mixture, prior to compression to a tablet, is not mushy.
  • a second embodiment of the invention is the treatment of a phosphate, per se, with caustic.
  • Phosphate and caustic in this embodiment have the same definitions as in the aforementioned first embodiment.
  • the formation of undesirable needle-like crystals is prevented by treating the phosphate with at least 4% caustic, such as sodium hydroxide.
  • caustic such as sodium hydroxide.
  • the percentage of caustic is based in part on equivalents of Na O.
  • the percentage of caustic is also based in part on the weight of the phosphate. In order to provide the required concentration of 23.5% as NaOH, about 4% to about 26% water, based on the weight 'of the phosphate, is employed with the caustic.
  • the treatment of the phosphate with caustic may have either one of two desired effects in this second embodiment. Firstly, it may promote or permit the growth of plate-like crystals in the phosphate rather than needle-like crystals. This is accomplished by using at least the minimum amount of caustic, i.e., 4%. Secondly, the phosphate may be treated with an even greater amount of caustic to preclude any crystal formation therein including both the needle-like crystals and also the plate-like crystals.
  • the treated phosphate of the second embodiment with plate-like crystals has utility as shown above in detergent tablets.
  • the treated phosphate without any crystals therein also has utility since it may be used in other detergent composition-s besides tablets, such as powders and flakes.
  • the present invention has a third embodiment.
  • the third embodiment is concerned with a detergent tablet containing a phosphate and a detergent having plate-like crystals therein without the caustic of the first embodiment.
  • the definitions for phosphate and detergents are the same as in the first embodiment.
  • the proportions of the essential phosphate and detergent components and the optional components are also the same as in the first embodiment.
  • a phosphate which does not have acid decomposition products thereon, may be combined with a detergent, e.g., an anionic detergent and a cationic detergent, to provide a detergent tablet also having high initial strength after compression and having the ability to dissolve quickly in water. Since there are no acid decomposition products, the tablet has desirable plate-like crystals rather than undesirable needle-like crystals.
  • a detergent e.g., an anionic detergent and a cationic detergent
  • a preferred tablet is one provided from a nonionic detergent and a phosphate. It has been found that this tablet does not dissolve or disintegrate in boiling alcohol, e.g., 300 ml. absolute ethyl alcohol which is allowed to boil for about five minutes. This is surprising since a tablet containing an anionic detergent and phosphate does dissolve and disintegrate in boiling alcohol and since the nonionic detergent, per se, is soluble in alcohol.
  • Example I Detergent tablets were prepared from the formulations indicated in Table I. This was accomplished by incorporating powdered phosphate and sodium sulfate into a revolving drum. A first liquid mixture of Sterox DJ and Pluronic F68 was then sprayed into the drum over an 8-10 minute period. Subsequently, a second liquid mixture of the sodium hydroxide, silicate and water was sprayed into the drum over an 8-10 minute period to agglomerate the particles therein. The agglomerated granules therefrom were screened by passing them through an 810 mesh screen. The screened granules were compressed thereafter in a die of a Stokes Duplex press at a pressure of about 500 psi. to form tablets.
  • the initial (fresh) strength of the tablets after compression was determined by the fracture strength test described above for the Black and Gray tablets.
  • the fraction strength of the tablets after they were cooled and stored thereafter for 24 hours was also determined. The results of these tests are also indicated in Table I.
  • Example II Tablets were prepared in a similar manner as described for Example I with the formulations listed in Table II.
  • the sodium carboxymethylcellulose was added initially to the drum with the powdered phosphate and sulfate.
  • a tablet with a relatively low initial strength after compression may be provided from a phosphate and a detergent indicating undesirable needle-like crystals therein.
  • a tablet is formed with a relatively high initial strength after compression indicating desirable plate-like crystals in the tablet. If less than Example III shows that using more than the critical amount of caustic will have an adverse effect in providing a detergent tablet. This is due to the fact that too much caustic will preclude the formation of desirable platelike crystals.
  • Example IV The procedures, described above for Example II, for preparing and testing tablets were repeated with the formulations in Table IV.
  • the critical amount and concentration of caustic is used, however, the initial strength of the compressed tablet is still relatively low since the tablet has the undesirable needle-like crystals rather than the desirable plate-like crystals therein.
  • Example III TABLE III Formulation Ingredients: (pounds) Pentasodium tripolyphosphate, Type I 2100.000 Sodium sulfate 518.000 Sodium carboxymethylcellulose 26.100 Sterox DJ 157.200 Pluronic F-68 174.600 Fluorescent dye 7.000 Sodium silicate solution at 46.6% solids (Na O-2.4SiO 487.000 Colorant 0.042 Perfume 3.950 NaOH (50%) 88.500
  • a tablet with a relatively low initial strength after compression may be formed because there are undesirable needle-like crystals therein.
  • a tablet with a relatively high initial strength after compression is formed by using a critical amount and concentration of caustic to prevent the formation of undesirable needle-like crystals but to permit or promote the formation of desirable plate-like crystals.
  • the tablets from formulations 2 and 3 in Example IV were also tested to determine their rate of disintegration and solubilization.
  • the tablets, 40 at a time were placed in a washing machine and agitated with water at 100 F. for seconds. Almost all of the tablets had completely disintegrated and dissolved after this time period.
  • a detergent tablet of this invention Besides having a relatively high initial strength, a detergent tablet of this invention, as shown in Example IV, disintegrates rapidly in water.
  • a detergent tablet having a high initial strength after compression and having the ability to disintegrate and dissolve rapidly in water which consists essentially of about 4% to about 13% of a synthetic organic nonionic detergent, about 5% to about of a phosphate which is selected from the group consisting of pentasodium tripolyphosphate, pentapotassium tripolyphosphate and mixtures thereof, 0.48% to 2.6% caustic which is a source of Na O or K 0, which is capable of forming a solution in water with a concentration based on equivalents of Na O of at least 23.5% as NaOH and which is selected from the group consisting of sodium hydroxide, potassium hydroxide, alkali metal silicates and mixtures thereof, and 2% to 11% water in order that there is a concentration of at least said 23.5 caustic in water.
  • a process for preparing detergent tablets having high initial strength after compression and having the ability to disintegrate and dissolve rapidly in water which comprises mixing together about 4% to about 13% of a synthetic organic nonionic detergent, about 5% to about 95 of a phosphate which is selected from the group consisting of pentasodium tripolyphosphate, pentapotassium tripolyphosphate and mixtures thereof, 0.48% to 2.6% caustic which is a source of Na O or K 0, which is capable of forming a solution in water with a concentration based on equivalents of Na O of at least 23.5% as NaOH and which is selected from the group consisting of sodium hydroxide, potassium hydroxide, alkali metal silicates and mixtures thereof, and 2% to 11% water in order that there is a concentration of at least said 23.5% caustic in water; and compressin the mixture at a pressure necessary to form tablets.
  • a synthetic organic nonionic detergent about 5% to about 95 of a phosphate which is selected from the group consisting of pen
  • a process for preparing detergent tablets having high initial strength after compression and having the ability to disintegrate and dissolve rapidly in water which comprises mixing together about 4% to about 13% of a synthetic organic nonionic detergent, about 20% to about 95% of pentasodium tripolyphosphate, 0.48% to 2.6% caustic which is a source of Na O or K 0, which is capable of forming a solution in water with a concentration based on equivalents of Na O of at least 23.5% as NaOH and which is selected from the group consisting of sodium hydroxide, potassium hydroxide, alkali metal silicates and mixtures thereof, and 2% to 11% water in order that there is a concentration of at least said 23.5% caustic in water until granules are formed; passing the granules through an 53-10 mesh screen; and compressing the screened granules into tablets at a pressure of about 200 to 5000 pounds per square inch using compressive forces rotating around the axis of compression with respect to the tablet being formed to effect a shearing force
  • a detergent tablet having a high initial strength after compression and havin the ability to disintegrate and dissolve rapidly in water which comprises 4.5% of the condensation product of 1 mole of dodecyl phenol with an average of 10 moles of ethylene oxide, 5.0% of HO 2 4 a s s b (CZHIIO c in which (C H O) represents a molcular weight of 1501- 1800 and n+ is an integer such that the molecule contains 8090% ethylene oxide, 60% of pentasodium tripolyphosphate with 20% as Form I and 80% as Form II, 6.5% of Na O-2.5SiO 0.3% of NaOH, 15.7% of sodium sulfate and 8.0% water; said tablet having Na o equivalents of 1.9% and having 25.6% concentration of total NaOH in water.
  • a detergent tablet having a high initial strength after compression and having the ability to disintegrate and dissolve rapidly in water whichcomprises 4.5% of the condensation product of 1 mole of dodecyl phenol with an average of moles of ethylene oxide, 5.0% of HO(C H O) (C H O) (C H O) I-I in (C3H 0) represents a molecular weight of 1501-1800 and a+c is an integer such that the molecule contains -90% ethylene oxide, 59.7% of pentasodium tripolyphosphate with 20% as Form I and 80% as Form II, 6.5% of Na O-2.5- SiO 0.28% of NaOH, 14.7% of sodium sulfate, 0.56% of sodium carboxymethylcellulose and 8.76% of water; said tablet having Na O equivalents of 2.12% and having a 24.2% concentration of total NaOH in water.
  • a detergent tablet having a high initial strength after compression and having the ability to disintegrate and dissolve rapidly in water which comprises 45% of the condensation product of 1 mole of dodecyl phenol with an average of 10 moles of ethylene oxide, 5.0% of HO(C H4O) ,(c3H5O) (C2H4O) H in (C3H 0)b represents a molecular weight of 150l1800 and a+c is an integer such that the molecule contains 8090% ethylene oxide, 59.6% of pentasodium tripoylphosphate with 20% as Form I and 80% as Form II, 6.5% of Na O-2.5- SiO 0.28% of NaOH, 14.7% of sodium sulfate, 0.56% of sodium carboxymethylcellulose and 8.86% water; said tablet having Na O equivalents of 2.13% and having a 24.2% concentration of total NaOH in water.
  • the caustic is a mixture of NaOH and Na O-ZASiO 11.
  • the detergent tablet according to claim 1 in which the phosphate is substituted with an amount up to 50% of trisodium orthophosphate, an amount up to 20% of tetrasodium pyrophosphate, an amount up to 20% of tetrapotassium pyrophosphate or an amount up to 30% of pentasodium tripoly-phosphate hexahydrate.

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US625884A 1963-12-31 1967-03-24 Treated phosphates Expired - Lifetime US3417024A (en)

Priority Applications (8)

Application Number Priority Date Filing Date Title
CH1670564A CH471891A (de) 1963-12-31 1964-12-28 Verfahren zur Herstellung einer Reinigungsmitteltablette
SE15744/64A SE306982B (de) 1963-12-31 1964-12-29
DEU11325A DE1296297B (de) 1963-12-31 1964-12-29 Nicht mit Silikaten beschichtete Reinigungsmitteltablette
DK642564AA DK116612B (da) 1963-12-31 1964-12-30 Vaskemiddel i tabletform.
GB52782/64A GB1093420A (en) 1963-12-31 1964-12-30 A detergent tablet
FR439A FR1420795A (fr) 1963-12-31 1964-12-30 Pains de détergent
BE657846A BE657846A (de) 1963-12-31 1964-12-31
US625884A US3417024A (en) 1963-12-31 1967-03-24 Treated phosphates

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US33473463A 1963-12-31 1963-12-31
US625884A US3417024A (en) 1963-12-31 1967-03-24 Treated phosphates

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US625884A Expired - Lifetime US3417024A (en) 1963-12-31 1967-03-24 Treated phosphates

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US (1) US3417024A (de)
BE (1) BE657846A (de)
CH (1) CH471891A (de)
DE (1) DE1296297B (de)
DK (1) DK116612B (de)
FR (1) FR1420795A (de)
GB (1) GB1093420A (de)
SE (1) SE306982B (de)

Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4219436A (en) * 1977-06-01 1980-08-26 The Procter & Gamble Company High density, high alkalinity dishwashing detergent tablet
US4370250A (en) * 1976-12-06 1983-01-25 Colgate-Palmolive Company Detergent tablet
US4451386A (en) * 1976-12-06 1984-05-29 Colgate-Palmolive Company Detergent tablet
EP0126963A1 (de) * 1983-05-02 1984-12-05 Henkel Kommanditgesellschaft auf Aktien Verfahren zur Herstellung von Reinigungsmitteltabletten
US4569780A (en) * 1978-02-07 1986-02-11 Economics Laboratory, Inc. Cast detergent-containing article and method of making and using
US4687121A (en) * 1986-01-09 1987-08-18 Ecolab Inc. Solid block chemical dispenser for cleaning systems
US4690305A (en) * 1985-11-06 1987-09-01 Ecolab Inc. Solid block chemical dispenser for cleaning systems
USRE32763E (en) * 1978-02-07 1988-10-11 Ecolab Inc. Cast detergent-containing article and method of making and using
USRE32818E (en) * 1978-02-07 1989-01-03 Ecolab Inc. Cast detergent-containing article and method of using
US5078301A (en) * 1987-10-02 1992-01-07 Ecolab Inc. Article comprising a water soluble bag containing a multiple use amount of a pelletized functional material and methods of its use
US5133892A (en) * 1990-10-17 1992-07-28 Lever Brothers Company, Division Of Conopco, Inc. Machine dishwashing detergent tablets
WO1993001266A1 (en) * 1991-07-03 1993-01-21 Winbro Group, Ltd. Cake-like detergent and method of manufacture
US5234615A (en) * 1987-10-02 1993-08-10 Ecolab Inc. Article comprising a water soluble bag containing a multiple use amount of a pelletized functional material and methods of its use
US5318713A (en) * 1992-06-08 1994-06-07 Binter Randolph K Solid detergent composition with multi-chambered container
US5552079A (en) * 1993-09-13 1996-09-03 Diversey Corporation Tableted detergent, method of manufacture and use
EP0839906A1 (de) * 1996-11-01 1998-05-06 Unilever Plc Waschmittelzusammensetzung
WO2000012671A1 (en) * 1998-08-28 2000-03-09 The Procter & Gamble Company Detergent tablet
FR2784392A1 (fr) * 1998-10-09 2000-04-14 Rhodia Chimie Sa Tablettes de composition detergente ou anticalcaire et leur mise en oeuvre en lave-vaisselle ou lave-linge
US6372707B1 (en) 1997-06-06 2002-04-16 Lever Brothers Company, Division Of Conopco, Inc. Cleaning compositions
US6506720B1 (en) 1997-03-13 2003-01-14 Henkel Kommanditgesellschaft Auf Aktien Process for preparing household detergent or cleaner shapes
US7008912B1 (en) 1997-03-11 2006-03-07 Henkel Kgaa Pressed piece which disintegrates in liquids

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB8830010D0 (en) * 1988-12-22 1989-02-15 Unilever Plc Detergent composition
DE19749749A1 (de) * 1997-11-11 1999-05-12 Henkel Kgaa Verfahren zur Herstellung stabiler und schnell zerfallender Waschmittelformkörper
GB2367830A (en) * 2000-10-12 2002-04-17 Procter & Gamble Process for preparing tablets

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1050005B (de) * 1956-05-15
US2811419A (en) * 1953-03-21 1957-10-29 Knapsack Ag Process for producing monomeric phosphates
US2909490A (en) * 1954-07-28 1959-10-20 Olin Mathieson Manufacture of duplex composition of sodium tripolyphosphate and sodium silicate solution
US2961410A (en) * 1957-04-02 1960-11-22 Procter & Gamble Process for preparing detergent compositions
US2987483A (en) * 1956-07-02 1961-06-06 Pennsalt Chemicals Corp Cleaning composition
US3081267A (en) * 1959-12-31 1963-03-12 Procter & Gamble Detergent tablet and process for making same
US3174934A (en) * 1961-04-24 1965-03-23 Monsanto Co Hydration of sodium tripolyphosphate

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3231506A (en) * 1961-04-03 1966-01-25 Colgate Palmolive Co Process for making detergent tablet
NL289572A (de) * 1962-03-07

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2811419A (en) * 1953-03-21 1957-10-29 Knapsack Ag Process for producing monomeric phosphates
US2909490A (en) * 1954-07-28 1959-10-20 Olin Mathieson Manufacture of duplex composition of sodium tripolyphosphate and sodium silicate solution
DE1050005B (de) * 1956-05-15
US2987483A (en) * 1956-07-02 1961-06-06 Pennsalt Chemicals Corp Cleaning composition
US2961410A (en) * 1957-04-02 1960-11-22 Procter & Gamble Process for preparing detergent compositions
US3081267A (en) * 1959-12-31 1963-03-12 Procter & Gamble Detergent tablet and process for making same
US3174934A (en) * 1961-04-24 1965-03-23 Monsanto Co Hydration of sodium tripolyphosphate

Cited By (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4370250A (en) * 1976-12-06 1983-01-25 Colgate-Palmolive Company Detergent tablet
US4451386A (en) * 1976-12-06 1984-05-29 Colgate-Palmolive Company Detergent tablet
US4219436A (en) * 1977-06-01 1980-08-26 The Procter & Gamble Company High density, high alkalinity dishwashing detergent tablet
US4569780A (en) * 1978-02-07 1986-02-11 Economics Laboratory, Inc. Cast detergent-containing article and method of making and using
USRE32763E (en) * 1978-02-07 1988-10-11 Ecolab Inc. Cast detergent-containing article and method of making and using
USRE32818E (en) * 1978-02-07 1989-01-03 Ecolab Inc. Cast detergent-containing article and method of using
EP0126963A1 (de) * 1983-05-02 1984-12-05 Henkel Kommanditgesellschaft auf Aktien Verfahren zur Herstellung von Reinigungsmitteltabletten
US4690305A (en) * 1985-11-06 1987-09-01 Ecolab Inc. Solid block chemical dispenser for cleaning systems
US4687121A (en) * 1986-01-09 1987-08-18 Ecolab Inc. Solid block chemical dispenser for cleaning systems
US5078301A (en) * 1987-10-02 1992-01-07 Ecolab Inc. Article comprising a water soluble bag containing a multiple use amount of a pelletized functional material and methods of its use
US5234615A (en) * 1987-10-02 1993-08-10 Ecolab Inc. Article comprising a water soluble bag containing a multiple use amount of a pelletized functional material and methods of its use
US5133892A (en) * 1990-10-17 1992-07-28 Lever Brothers Company, Division Of Conopco, Inc. Machine dishwashing detergent tablets
US5209864A (en) * 1991-07-03 1993-05-11 Winbro Group, Ltd. Cake-like detergent and method of manufacture
WO1993001266A1 (en) * 1991-07-03 1993-01-21 Winbro Group, Ltd. Cake-like detergent and method of manufacture
US5318713A (en) * 1992-06-08 1994-06-07 Binter Randolph K Solid detergent composition with multi-chambered container
US5552079A (en) * 1993-09-13 1996-09-03 Diversey Corporation Tableted detergent, method of manufacture and use
EP0839906A1 (de) * 1996-11-01 1998-05-06 Unilever Plc Waschmittelzusammensetzung
US7008912B1 (en) 1997-03-11 2006-03-07 Henkel Kgaa Pressed piece which disintegrates in liquids
US6506720B1 (en) 1997-03-13 2003-01-14 Henkel Kommanditgesellschaft Auf Aktien Process for preparing household detergent or cleaner shapes
USRE39139E1 (en) * 1997-03-13 2006-06-20 Henkel Kgaa Process for preparing household detergent or cleaner shapes
US6372707B1 (en) 1997-06-06 2002-04-16 Lever Brothers Company, Division Of Conopco, Inc. Cleaning compositions
WO2000012671A1 (en) * 1998-08-28 2000-03-09 The Procter & Gamble Company Detergent tablet
FR2784392A1 (fr) * 1998-10-09 2000-04-14 Rhodia Chimie Sa Tablettes de composition detergente ou anticalcaire et leur mise en oeuvre en lave-vaisselle ou lave-linge
WO2000022090A1 (fr) * 1998-10-09 2000-04-20 Rhodia Chimie Tablettes de composition detergente ou anticalcaire et leur mise en oeuvre en lave-vaisselle ou lave-linge
AU754500B2 (en) * 1998-10-09 2002-11-21 Rhodia Chimie Detergent and descaling composition tablets and use in dishwasher and washing machine

Also Published As

Publication number Publication date
CH471891A (de) 1969-04-30
BE657846A (de) 1965-06-30
FR1420795A (fr) 1965-12-10
DK116612B (da) 1970-01-26
DE1296297B (de) 1969-05-29
SE306982B (de) 1968-12-16
GB1093420A (en) 1967-11-29

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