CA1173323A - Agglomeration process for making granular detergents - Google Patents
Agglomeration process for making granular detergentsInfo
- Publication number
- CA1173323A CA1173323A CA000398237A CA398237A CA1173323A CA 1173323 A CA1173323 A CA 1173323A CA 000398237 A CA000398237 A CA 000398237A CA 398237 A CA398237 A CA 398237A CA 1173323 A CA1173323 A CA 1173323A
- Authority
- CA
- Canada
- Prior art keywords
- composition
- added
- sodium
- alkali metal
- caking
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
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Classifications
-
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/06—Phosphates, including polyphosphates
- C11D3/062—Special methods concerning phosphates
-
- 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/72—Ethers of polyoxyalkylene glycols
-
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/046—Salts
-
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/08—Silicates
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Detergent Compositions (AREA)
Abstract
AGGLOMERATION PROCESS FOR MAKING
GRANULAR DETERGENTS
Abstract of the Disclosure Granular detergent compositions resistant to caking in dispenser cups are prepared by the addition of water or an aqueous sodium sili-cate solution agglomerating agent to particulate ingredients compris-ing sodium tripolyphosphate followed by the addition of an alkali metal chloride having a particle size such that at least 75% by weight passes through a 35 Tyler mesh screen after at least about 30% of said agglomerating agent has been added to said particulate ingredients.
GRANULAR DETERGENTS
Abstract of the Disclosure Granular detergent compositions resistant to caking in dispenser cups are prepared by the addition of water or an aqueous sodium sili-cate solution agglomerating agent to particulate ingredients compris-ing sodium tripolyphosphate followed by the addition of an alkali metal chloride having a particle size such that at least 75% by weight passes through a 35 Tyler mesh screen after at least about 30% of said agglomerating agent has been added to said particulate ingredients.
Description
~L 173323 .
AGGLOMERATION PR~CESS FOR MAKING
GRANULAR DETERGENTS
;'`
Background of the Invention Field of the Invention This invention relates to a process for making a gran-ular detergent product and the product of the process. More particularly, the invention relates to a process for preparing detergent compositions which are useful in automatic dish-washing machines.
State of the Art ; Detergent compositions comprising in combination an alkali metal polyphosphate such as sodium tripolyphosphate, alkaline ~alts such as sodium silicate and sodium carbonate, a surfactant and a chlorine containing compound that provides hypochlorite ion in solution have particular utility for machine dishwashing. The production of such compositions made of agglomerates of the ingredients has generally been accomplished by the addition of water or an aqueous sodium silicate solution to a mixture of dry ingredients. Compositions prepared in such ; manner, however, are characteri2ed by a tendency to cake in ~- their cartons during storage and can also have a tendency to cake in the dispenser cups of automatic dishwashing machines.
A number of process modifications have been suggested to reduce the caking tendency of detergent compositions prepared using water or silicate solutions as agglomerating agents. U.S. Patent
AGGLOMERATION PR~CESS FOR MAKING
GRANULAR DETERGENTS
;'`
Background of the Invention Field of the Invention This invention relates to a process for making a gran-ular detergent product and the product of the process. More particularly, the invention relates to a process for preparing detergent compositions which are useful in automatic dish-washing machines.
State of the Art ; Detergent compositions comprising in combination an alkali metal polyphosphate such as sodium tripolyphosphate, alkaline ~alts such as sodium silicate and sodium carbonate, a surfactant and a chlorine containing compound that provides hypochlorite ion in solution have particular utility for machine dishwashing. The production of such compositions made of agglomerates of the ingredients has generally been accomplished by the addition of water or an aqueous sodium silicate solution to a mixture of dry ingredients. Compositions prepared in such ; manner, however, are characteri2ed by a tendency to cake in ~- their cartons during storage and can also have a tendency to cake in the dispenser cups of automatic dishwashing machines.
A number of process modifications have been suggested to reduce the caking tendency of detergent compositions prepared using water or silicate solutions as agglomerating agents. U.S. Patent
2,895,916 discloses an order of additon in which chlorinated : , trisodium phosphate is added to the composition only after the aqueous silicate has been added to an anhydrous polyphosphate.
A carton caking benefit is said to result from a more rapid hydration of the sodium tripolyphosphate in the absence of chlor~nated trisodium phosphate.
.....
It has now been found that a substantial reduction in the dispenser cup caking tendency of agglomerated detergent compositionS containing sodium tripoIyphosphate, an alkali metal silicate and a low-foaming nonionic surfactant can be ~- achieved if from about 2~ to about 20~ of certain alkali metal : 35 salts are added to the detergent composition after -~ the agglomeration step comprising the addition of 1 ~73323 :. :~ , ,.
.
. water or an aqueous alkali metal silicate solution to a particulate mixture comprising sodium tripolyphosphate has commenced and prefer-ably is substantially complete.
It is an object of this invention to produce agglomerated granular de-tergent compositions which are resistant to caking ;n dispenser cups.
ûther objects and advantages will be apparent from the ~ollowing - description and examples.
Summary of the Invention ~; The invention is the composition of and the process ~or an agglom-erated granular detergent comprising from about 15% to about 50% of sodium tripolyphosphate, from about 5% to about 25% silicate solids wherein the average SiO2:M20 ~eight ratio is from about 1.0 ~to about 3.G, M being an alkali metal, Prom about 2% to about 12% of a low-foaming nonionic surfac-tant and from about 2% to about 20% oF a dispenser cup caking inhibitor selected from the group consisting of alkali metal chlorides and mixtures thereof, said dispenser cup caking inhibitor being a dry material having a particle size such that at lea~t about 83% passes through a 35 Tyler mesh screen, said agglom-- erated granular detergent composition produced by agitating particu-late components comprising anhydrous sodiu~ tripolyphosphate, contacting said particulate components during said agitating with an agglomerating agent comprising water, mixing said agglomerating agent with said particulate components by continuing said agitating, adding said dispenser cup caking inhibitor during said agitating after at ' '.;t,. 25 least about ~0% and preferably at least about 75% of said agglomera-ting agent has been added to said particulate components and recover-ing said agglomerated granular detergent composition.
Detailed Description of the Invention The process of the invention is carried out in apparatus sui-table for the m:ixing of dry particulate components and adapted so that liquid components such as water or an aqueous alkali metal siiicate solution agglomerating agent can b~ sprayed on or otherwise added to a bed or falling curtain of one or more particulate components during the mixing operation. Any suitable mixing device such as an inclined pan agglomer~tor, a rotating drum or any other vessel with suitable means of agitation m~y be used. Methads oF agitating, mixing and agglomerating particulate components are ~ell known to those skilled :.
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i in the art. The apparatus may be designed or adapted for either con-;~,...
,~,; tinuous or batch operation so long as the essential process steps can ~ be achieved.
... :. , Optional process steps include screening of particulate materials before processing, screening or grinding the composit;on to any de-, *, .
sired particle size, addition of optional ingredients such as an ;~ alkali metal dichlorocyanurate bleach and sodium carbonate, and allow-ing the final composition to come to equilibrium with respect to tem-perature and hydration before packing into cartons.
10The theoretical basis for the unexpected improvement in dispenser ~ cup caking resistance provided by incorporation of the dispenser cup - -. caking inhibitor is believed to be at least partially related to ~he complex hydration characteristics of anhydrous sodium tripolyphos-~` phate. This compound has different hydration characteristics depend-ing on its method of manufacture. A so-called Form I is produced if the process of manufacture includes a relatively high temperature calcination step. A Form II results when lower temperatures are employed. Form I is characterized by relatively rapid hydration char-acteristics. Form II, particularly in the absence of any substantial level of Form I material, is slow to hydrate, but h~s a greater immediate solubility. Commercially available sodium tripolyphosphate ~; is generally a mixture of Form I and Form II. U.S. Patents 2,622,058, 2,961,40g and 2,961941û disclose the hydration characteristics of Form I and Form II sodium tripolyphosphate in the manufac-~ ,d~ 23 ture of spray-dricd detergents.
i The process and product of this invention apply to granular deter-gent compositions comprising the following essential ingredients: (1) ; , sodium tripolyphosphate; (2) alkali metal silicate; (3) a low-foaming ~ nonionic surfactant; and (4) an alkali metal salt dispenser cup caking ~ 30 inhibitor.
Sodium Tripolyphosphate The deterg-nt compositions of the invention contain sodium tri-~' polyphosphate at a level of from about 15% to about 50% and preferably ,: from about 25% to about 45% by weight.
35Anhydrous sodium tripolyphosphate comprises all or a part of the particulate components contacted with the agglomerating agent in the process aspect of the invention. The sodium tripolyphosphate can be ....
~. ~ 73323 . .
in granular form such that at least about 90% is retained on a 100 Tyler mesh screen or in powdered form such that at least about 90%
- passes through a 100 Tyler mesh screen Optional polyphosphates useful in -the practice of the invention are the water-soluble sodium and potassium salts of pyrophosphoric acid (H4P207~ and polymeric metaphosphoric acid (HP03)n. The value of n is typically below about 50 in the interest of water solu-bility. The sodium and potassium salts o~ metaphosphoric acid are often designated "glassy" phosphates and exist as a series of polymers. Glassy phosphates may also be represented by the formula -~ ~M2û)m(P205)n wherein M is an alkali metal, n is in the range of- from about 5 to about 50 and m:n is in the range of 1:1 to 1:1.5 on a molar basis. An example of a glassy phosphate is sodium hexametaphos-phate (Na6P6ûl8).
~5 The Alkali Metal Silica-te The compositions made by the process of this invention contain , ,: alkali metal silicate solids at a level of from about 5% to about 25%
on an anhydrous weight basis and having an average SiO2:M2û weight ratio of from about l.û to about 3.6, M being an alkali metal. Parti-cularly preferred is a sodium silicate having a weight ratio of , SiO2LNa20 of from about 1.6 to about 3.3, most preferably from ~- , about 2 to about 3.2. Lower rat;o silicates which are relatively more - ,~ alkaline provide good cleaning performance but in order to provide , l, protection to materials such as aluminum and chlna, it is desi-rable to , , ; 25 have at least 10% and up to 75% of the SiO2 present at a SiO2:Na2û ratio above 3.Q. It is possible to add all of the sili-cate in the Form of aqueous solutions typically containing from about 35% to about 55% silicate solids but all or a portion may be part of ,~ the particulate components comprising sodium tripolyphosphate or added ,; 30 in dry form at some other point in the process. Aqueous alkali metal silicate solutions used as agglomerating agents preferably contain at least about ~5% water.
, , Silicate solids in the compositions of the invention can be added , dry in anhydrous or hydrous form. Preferably at least a portion of ; ,35 the total silicate is hydrous silicate mixed with sodium tripolyphos-phate ~efore the addition of an agglomeration agent, ~,'~ ,, x~
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~ Low-Foaminq Nonionic Surfactant . . ~
~ he compositions of this invention con-tain from about 2.0% to about 12% of a low-foaming nonionic surFactant by weight. A preferred level of surfactant is from about 3.0% to about 8.0%. Preiferably the surfactant is an alkoxylated nonionic surfactant and preferably the ` composition is essentially free of- sulfonated or sulfated anionic -; surfactants.
- Examples of nonionic surfactants include:
~ ) the condensation product of 1 mole of a saturated or unsatur-; 10 ated, straight or branched chain, alcohol or fatty acid con-taining from about 10 to about 20 carbon atoms with from _ about 4 to about 50 moles of ethylene oxide. Specific i~ examples of such compounds include a condensation product af 1 mole of coconu-t fatty acid or tallow fatty acid with 10 moles of ethylene oxide; the condensation of 1 mole of oleic acid with 9 moles of ethylene oxide; the condensation product Ç ~ of 1 mole of stearic acid with 25 moles of ethylene oxide;
the condensation product of 1 mole of tallow fatty alcohols ~ with about 9 moles of ethylene oxide; the condensation Yi- ~ - 20 product o~ 1 mole of oleyl alcohol with 10 moles of ethylene oxide; the condensation product of 1 mole of Clg alcohol and 8 moles of ethylene oxide; and the condensation product ~ ~ of one mole of C18 alcohol and 9 moles of ethylene oxide.
t`:: ~he condensation product of a fatty alcohol containing ~` 25 from 17 to 19 carbon atoms, and being substantially free of chain leng-ths above and below these numbers, with from about 6 to about 15 moles, preferably 7 to 12 moles, most prefer-ably 8 moles, of ethylene ox;de is particularly preferred ' !." This can be capped with a low molecular weight (Cl 5) acid I 30 or alcohnl moiety, so as to minirnize or eliminate the need "-"r-~ for a suds-suppressing agent.
(2) Polyethylene glycols having molecular weights of from about 1,400 to about 30,00û, e.g., 20,000; 9,500; 7,500; 6,000;
4,500; 3,400; and 1,450. All of these materials are waxlike solids which melt between 110F and 200F.
A carton caking benefit is said to result from a more rapid hydration of the sodium tripolyphosphate in the absence of chlor~nated trisodium phosphate.
.....
It has now been found that a substantial reduction in the dispenser cup caking tendency of agglomerated detergent compositionS containing sodium tripoIyphosphate, an alkali metal silicate and a low-foaming nonionic surfactant can be ~- achieved if from about 2~ to about 20~ of certain alkali metal : 35 salts are added to the detergent composition after -~ the agglomeration step comprising the addition of 1 ~73323 :. :~ , ,.
.
. water or an aqueous alkali metal silicate solution to a particulate mixture comprising sodium tripolyphosphate has commenced and prefer-ably is substantially complete.
It is an object of this invention to produce agglomerated granular de-tergent compositions which are resistant to caking ;n dispenser cups.
ûther objects and advantages will be apparent from the ~ollowing - description and examples.
Summary of the Invention ~; The invention is the composition of and the process ~or an agglom-erated granular detergent comprising from about 15% to about 50% of sodium tripolyphosphate, from about 5% to about 25% silicate solids wherein the average SiO2:M20 ~eight ratio is from about 1.0 ~to about 3.G, M being an alkali metal, Prom about 2% to about 12% of a low-foaming nonionic surfac-tant and from about 2% to about 20% oF a dispenser cup caking inhibitor selected from the group consisting of alkali metal chlorides and mixtures thereof, said dispenser cup caking inhibitor being a dry material having a particle size such that at lea~t about 83% passes through a 35 Tyler mesh screen, said agglom-- erated granular detergent composition produced by agitating particu-late components comprising anhydrous sodiu~ tripolyphosphate, contacting said particulate components during said agitating with an agglomerating agent comprising water, mixing said agglomerating agent with said particulate components by continuing said agitating, adding said dispenser cup caking inhibitor during said agitating after at ' '.;t,. 25 least about ~0% and preferably at least about 75% of said agglomera-ting agent has been added to said particulate components and recover-ing said agglomerated granular detergent composition.
Detailed Description of the Invention The process of the invention is carried out in apparatus sui-table for the m:ixing of dry particulate components and adapted so that liquid components such as water or an aqueous alkali metal siiicate solution agglomerating agent can b~ sprayed on or otherwise added to a bed or falling curtain of one or more particulate components during the mixing operation. Any suitable mixing device such as an inclined pan agglomer~tor, a rotating drum or any other vessel with suitable means of agitation m~y be used. Methads oF agitating, mixing and agglomerating particulate components are ~ell known to those skilled :.
-- ( w --:..``
..
i in the art. The apparatus may be designed or adapted for either con-;~,...
,~,; tinuous or batch operation so long as the essential process steps can ~ be achieved.
... :. , Optional process steps include screening of particulate materials before processing, screening or grinding the composit;on to any de-, *, .
sired particle size, addition of optional ingredients such as an ;~ alkali metal dichlorocyanurate bleach and sodium carbonate, and allow-ing the final composition to come to equilibrium with respect to tem-perature and hydration before packing into cartons.
10The theoretical basis for the unexpected improvement in dispenser ~ cup caking resistance provided by incorporation of the dispenser cup - -. caking inhibitor is believed to be at least partially related to ~he complex hydration characteristics of anhydrous sodium tripolyphos-~` phate. This compound has different hydration characteristics depend-ing on its method of manufacture. A so-called Form I is produced if the process of manufacture includes a relatively high temperature calcination step. A Form II results when lower temperatures are employed. Form I is characterized by relatively rapid hydration char-acteristics. Form II, particularly in the absence of any substantial level of Form I material, is slow to hydrate, but h~s a greater immediate solubility. Commercially available sodium tripolyphosphate ~; is generally a mixture of Form I and Form II. U.S. Patents 2,622,058, 2,961,40g and 2,961941û disclose the hydration characteristics of Form I and Form II sodium tripolyphosphate in the manufac-~ ,d~ 23 ture of spray-dricd detergents.
i The process and product of this invention apply to granular deter-gent compositions comprising the following essential ingredients: (1) ; , sodium tripolyphosphate; (2) alkali metal silicate; (3) a low-foaming ~ nonionic surfactant; and (4) an alkali metal salt dispenser cup caking ~ 30 inhibitor.
Sodium Tripolyphosphate The deterg-nt compositions of the invention contain sodium tri-~' polyphosphate at a level of from about 15% to about 50% and preferably ,: from about 25% to about 45% by weight.
35Anhydrous sodium tripolyphosphate comprises all or a part of the particulate components contacted with the agglomerating agent in the process aspect of the invention. The sodium tripolyphosphate can be ....
~. ~ 73323 . .
in granular form such that at least about 90% is retained on a 100 Tyler mesh screen or in powdered form such that at least about 90%
- passes through a 100 Tyler mesh screen Optional polyphosphates useful in -the practice of the invention are the water-soluble sodium and potassium salts of pyrophosphoric acid (H4P207~ and polymeric metaphosphoric acid (HP03)n. The value of n is typically below about 50 in the interest of water solu-bility. The sodium and potassium salts o~ metaphosphoric acid are often designated "glassy" phosphates and exist as a series of polymers. Glassy phosphates may also be represented by the formula -~ ~M2û)m(P205)n wherein M is an alkali metal, n is in the range of- from about 5 to about 50 and m:n is in the range of 1:1 to 1:1.5 on a molar basis. An example of a glassy phosphate is sodium hexametaphos-phate (Na6P6ûl8).
~5 The Alkali Metal Silica-te The compositions made by the process of this invention contain , ,: alkali metal silicate solids at a level of from about 5% to about 25%
on an anhydrous weight basis and having an average SiO2:M2û weight ratio of from about l.û to about 3.6, M being an alkali metal. Parti-cularly preferred is a sodium silicate having a weight ratio of , SiO2LNa20 of from about 1.6 to about 3.3, most preferably from ~- , about 2 to about 3.2. Lower rat;o silicates which are relatively more - ,~ alkaline provide good cleaning performance but in order to provide , l, protection to materials such as aluminum and chlna, it is desi-rable to , , ; 25 have at least 10% and up to 75% of the SiO2 present at a SiO2:Na2û ratio above 3.Q. It is possible to add all of the sili-cate in the Form of aqueous solutions typically containing from about 35% to about 55% silicate solids but all or a portion may be part of ,~ the particulate components comprising sodium tripolyphosphate or added ,; 30 in dry form at some other point in the process. Aqueous alkali metal silicate solutions used as agglomerating agents preferably contain at least about ~5% water.
, , Silicate solids in the compositions of the invention can be added , dry in anhydrous or hydrous form. Preferably at least a portion of ; ,35 the total silicate is hydrous silicate mixed with sodium tripolyphos-phate ~efore the addition of an agglomeration agent, ~,'~ ,, x~
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~, .
~ - 5 -":'`
~ Low-Foaminq Nonionic Surfactant . . ~
~ he compositions of this invention con-tain from about 2.0% to about 12% of a low-foaming nonionic surFactant by weight. A preferred level of surfactant is from about 3.0% to about 8.0%. Preiferably the surfactant is an alkoxylated nonionic surfactant and preferably the ` composition is essentially free of- sulfonated or sulfated anionic -; surfactants.
- Examples of nonionic surfactants include:
~ ) the condensation product of 1 mole of a saturated or unsatur-; 10 ated, straight or branched chain, alcohol or fatty acid con-taining from about 10 to about 20 carbon atoms with from _ about 4 to about 50 moles of ethylene oxide. Specific i~ examples of such compounds include a condensation product af 1 mole of coconu-t fatty acid or tallow fatty acid with 10 moles of ethylene oxide; the condensation of 1 mole of oleic acid with 9 moles of ethylene oxide; the condensation product Ç ~ of 1 mole of stearic acid with 25 moles of ethylene oxide;
the condensation product of 1 mole of tallow fatty alcohols ~ with about 9 moles of ethylene oxide; the condensation Yi- ~ - 20 product o~ 1 mole of oleyl alcohol with 10 moles of ethylene oxide; the condensation product of 1 mole of Clg alcohol and 8 moles of ethylene oxide; and the condensation product ~ ~ of one mole of C18 alcohol and 9 moles of ethylene oxide.
t`:: ~he condensation product of a fatty alcohol containing ~` 25 from 17 to 19 carbon atoms, and being substantially free of chain leng-ths above and below these numbers, with from about 6 to about 15 moles, preferably 7 to 12 moles, most prefer-ably 8 moles, of ethylene ox;de is particularly preferred ' !." This can be capped with a low molecular weight (Cl 5) acid I 30 or alcohnl moiety, so as to minirnize or eliminate the need "-"r-~ for a suds-suppressing agent.
(2) Polyethylene glycols having molecular weights of from about 1,400 to about 30,00û, e.g., 20,000; 9,500; 7,500; 6,000;
4,500; 3,400; and 1,450. All of these materials are waxlike solids which melt between 110F and 200F.
(3) The condensation products of 1 mole of alkyl phenol wherein ~, ; the alkyl chain contains from about 8 to abnut 18 carbon atoms and from about 4 to about 50 moles o-f ethylene oxide.
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~ 173323 Specific examples of these nonionics are the condensation products of 1 mole of decylphenol with 40 moles of ethylene oxide; tho condensation product of 1 mole of dodecylphenol with 3S moles of ethylene oxide; the condensation product of ~ - 5 1 mole of tetradecylphenol with 25 moles of ethylene oxide;
- the condensation product of 1 mole of heptadecylphenol with - 30 moles of ethylene oxide, etc.
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~ 173323 Specific examples of these nonionics are the condensation products of 1 mole of decylphenol with 40 moles of ethylene oxide; tho condensation product of 1 mole of dodecylphenol with 3S moles of ethylene oxide; the condensation product of ~ - 5 1 mole of tetradecylphenol with 25 moles of ethylene oxide;
- the condensation product of 1 mole of heptadecylphenol with - 30 moles of ethylene oxide, etc.
(4) Polyoxypropylene, polyoxyethylene condensates having the formula HO(C2H40)x(C3H60)y (C2H40)x H
where y equals at least 15 and (C2H40~x-~x equals 20Yo to 90% of the total weight of the compound and the molecular weight is from about 2,000 to about lû,OOO, preferably ~om `; about 3,0ûO to about 6,000. These materials are, for exam-i 15 ple, the PLURONIC~which are well known in the art.
. (5) The compounds of (1) which are capped with propylen- oxide, butylene oxide and/or short chain alcohols and/or short chain fatty acids, e.g., those containing from 1 to about 5 carbon - atoms, and mixtures thereof.
(6) Condensation produsts of ethylene oxide and propylenP oxide ~-; with a low molecular weight trifunctional alcohol such as glycerine or trimethylolproPane. These materials are9 for - example, the PLURADOT** polygols made by the BASF Wyandotte ~' Corporation.
Preferred surfactants are those having the formula Rû-(~2H4û)xRl wherein R is an alkyl or alkylene group .~ containing from 17 to 19 carbon atoms, x is a number From about 6 to about 15, preferably from about 7 to about 12, and Rl is selected from the group consisting of hydrogon, Cl 5 alkyl groups, C2 5 acyl groups and groups having the formula -(CyH2yû)nH wherein y ~ ~ is 3 to 4 and n is a number from 1 to about 4.
;~ Also preferred are the low sudsing compounds of (4), the oth~r compounds ~f t5), and C17 19 materials of (1) which have a nar-~ row ethoxy distribution.
`- 35 In addition to the above mentioned sorfactants, other suit2ble ~ surfactants can be found in the disclosure of U.S. Patents 3,544,473, r~ ' 3,63û,923, 3,8~8,781 and 4,0011132.
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~ 3 3 2 3 Alkali Metal Salt Dispenser Cup Caking Inhibitor The compositions of the invention contain from about 2% to about 20Yo~ preferably from about 4% to about 15%, of a dispencer cup caking .` inhibitor selected from the group consis-ting of alkali metal chlorides and mixtures thereof.
,.. ~ Operative dispenser cup caking inhibitors are in the form of dry `;~ powders having a particle size such that at least about 80% passes through a 3S Tyler mesh screen. The dispenser cup caking inhibitor is : added during the process of the inventi,on after at least about 30~0, , lO preferably about 75%, and most pre~erably about 90%, oF the water or "~ aqueous sodium silicate agglomerating agent has been added to the . ~;.
particulate cnmponents comprising sodium tripolyph~sphate.
. An especially preferred material is sodium chloride having a par-ticle size such that at least 8û% passes through a 100 Tyler mesh `` 15 screen.
s Water The compositions of the invention are made by a process in which ,'~,',5',' either water or an aqueous sodium silicate solution is used as the agglomerating agent.
- 20 The finished compositions will contain water in the form of hydra-, ted salts, preferably from about 9% to about 12% by weight.
, Alkali Metal Dichlorocyanurate . Sodium or potassium dichlorocyanurate is optionally but preferably ~, incorporated in the compositions of the invention in an am~unt suffi-, ,~ 25 cient to provide available chlorine equal to from about 0.75% to aboùt ,` 2.5% by weight of the composition. A preferred material is sodium dichlorocyanurate dihYdrate as disclosed in U~S. Patent 3~936~386 which provides 56% available chlorine by weight. The ability of a compound to provide hypochlorite ';;! 30 ion in solution is generally measured as "available chlorine". The . . .
, available chlorine reflects the m_thod of producing an inorganic hypo-; chlorite (e.g., 2 NaOH ~ C12 ~ NaOC1 ~ NaCl -~ H20). Avail-able chlorine is the chlorine liberated by acidification of a solution , , of hypochlorite ions and at least a molar equivalent amount of - , 35 chloride ions. The usual analytical method of determining available ,~ chlorine in a solution is addition of an excess of an iodide salt and ` titration of the liberated free iodine with a reducing agent.
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:~l'733~3 ODtional Alkali ~etal Car~onates Optionally, the process and composition of the invention utilize alkali metal carbonate to provide the alkalinity needed ; for optimum cleaning performance.
Alkali metal carbonates, particularly sodium carbonate, can be present in the compositions at levels up to about 25% prefer-ably from about 2% to about 12% by weight.
Other Optional ~ngredients In addition to the above ingredients it can be desirable, - : 10 if the product sudses too much, to incorporate one of the many suds-suppressing ingredients disclosed in the above mentioned patents at a level of from about 0.01% to about 10%, preferably from about 0.05% to about 3%. The preferred suds suppressing - .
` materials are mono- and distearyl acid phosphates; the self-, 15 emuIsified siloxane suds suppressors of U.S. Patent 4,126,045 ~;~. and mixtures thereof.
~` Organic se~uestering builders such as citrates and nitrilotriacetates can be present in the compositions, but preferably at levels no greater than about 10% by weight. The ~; 20 presence of organic builders tends to hurt the performance of ~i these compositions by leaving visible spots and filming on 1'` ~
s~ glassware.
China protecting agents including aluminosilicates, aluminates, ~, etc., can be present in amounts up to about 5%, preferably from about 0.2% to about 2%.
~ Filler materials, sodium sulfate in particular, to control s ; product density and other physical characteristics can also be ~: present in amounts up to about 60%, preferably not more than about 30~ by weight.
Dyes, perfumes, crystal modifiers and the like can also be added in rninor amounts.
As used herein, all percentages, parts and ratios are by ;; weight unless otherwise stated.
r' ~ The following Examples illustrate the invention and facilitate ` 35 facilitate its understanding :
:
.
' ~
~ .
`~.; . ~173323 ' :
....
EXAMPLE I
A. 33.1 Parts by weight of powdered anhydrous sodium tripolyphosphate and 8.0 parts by weight of hydrous sodium silicate (82~ solids, SiO2:Na20 weight ratio of 2.4) were added to a ribbon mixer. With - - 5 the mixer in operation the following ingredients were added during a `~' cycle time of 180 seconds.
., a) from 0 seconds to ~65 seconds--added as a spray ~ blend of 1~.8 parts of an aqueous sodium silicate solution ,~; containing 47.3% silica-te solids with a Si~2:Na20 weight ratio of 2.0 and 4.7 parts of an aqueous sodium silicate solution containing 37.5% silicate solids with a ,~;, SiO2:Na20 weight ratio of 3.2. This solution also con-tained minor amounts of perfume and clye.
-~ b) at 60 seconds--added dry 19.4 parts of sodium sulfate and 10.0 parts of sodium car-~` bonate.
c) from 60 seconds to 165 seconds--added as a spray 4.0 parts of a polyoxyalkylene nonionic surfactant (condensa-y ' .
tion product of C18 alcohol with average of 8.25 moles ~; 20 ethylene oxide).
d) at 145 seconds--added dry 5cO parts of sodium chloride h~ving a particle size such that at least 80~ passed through a lûO Tyler mesh screen.
e) after 180 seconds -,~ 25 Product is discharged from mixer.
f) 2.5 parts of sodium dichlorocyanurate dihydrate was added and ; mixed in after drying and aging of the product discharged from the mixer at step e).
B. The process of A was repeated with the elimination of step d).
24.4 Parts sodium sulfate added at step b) replaced the.sodium chlor-ide of step d).
~ The compositions were packed in airtight containers pending evalu-; ~ ation. Resistance to automatic dishwasher dispenser cup caking was ; measured as indicated in the table below.
''' ,' .~. -~ ' .
~ ~3323 :. :
-- 10 -- .
Dispenser Cup Caking Grade Compnsition A B
- Automa-tic Dishwasher "Hotpoint'l ( trademark) end of main wash 0.6 3.0 middle of rinse 0.1 1.1 end of rinse 0.0 0.5 " Frigidaire" ( trademark) end of main wash 0.1 2.8 middle of rinse 0.0 1.6 end of rinse 0.0 0.6 - . ... ~ 1 ~ scale of 0-8. 0 indicating complete removal of product ,~ ;from cup, 8 indicating cup full of product.
Composition A was superior to Composition B in resistance to dis-:15 penser cup caking. No Composition A remained in the dispenser cup at the end of the rinse cycle, the point of principal notice of dispenser cup caking.
EXAMPLE II
The process of Example I-A was repeated with the substitution of NaCl having a particle size such that 80% passed through a 35 Tyler -mesh screen and less than 20% passed through a 10~ Tyler mesh screen.
The resultant composition was superior to Composition B sf Example I
but slightly inferior to Composition A of Example I.
EXAMPLE III
,~ 25 The materials listed in the~table below were added to Composition ,~ B of Example I at the levels and process cycle time indicated. 30û
grams of each resultant composition was mixed with 100 grams of 100F distilled water and stirred in a 400 ml beaker. Viscosity of the product slurries was measured by a Brookfield spindle viscometer !' 30 (#4 spindle/6 rpm) after seven minutes.
The reduction in viscosity for each additive was found to be pre-dictive of the improvement in resistance to dispenser cup caking.
, .
, .
. ., ~, .
. . .
~' .
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- Dispenser Cup Caking Inhibitnr Viscosity (cps) None 28,000 1% NaCl--added at 165 sec. 22,500 2% NaCl--added at 165 sec. 14,000
where y equals at least 15 and (C2H40~x-~x equals 20Yo to 90% of the total weight of the compound and the molecular weight is from about 2,000 to about lû,OOO, preferably ~om `; about 3,0ûO to about 6,000. These materials are, for exam-i 15 ple, the PLURONIC~which are well known in the art.
. (5) The compounds of (1) which are capped with propylen- oxide, butylene oxide and/or short chain alcohols and/or short chain fatty acids, e.g., those containing from 1 to about 5 carbon - atoms, and mixtures thereof.
(6) Condensation produsts of ethylene oxide and propylenP oxide ~-; with a low molecular weight trifunctional alcohol such as glycerine or trimethylolproPane. These materials are9 for - example, the PLURADOT** polygols made by the BASF Wyandotte ~' Corporation.
Preferred surfactants are those having the formula Rû-(~2H4û)xRl wherein R is an alkyl or alkylene group .~ containing from 17 to 19 carbon atoms, x is a number From about 6 to about 15, preferably from about 7 to about 12, and Rl is selected from the group consisting of hydrogon, Cl 5 alkyl groups, C2 5 acyl groups and groups having the formula -(CyH2yû)nH wherein y ~ ~ is 3 to 4 and n is a number from 1 to about 4.
;~ Also preferred are the low sudsing compounds of (4), the oth~r compounds ~f t5), and C17 19 materials of (1) which have a nar-~ row ethoxy distribution.
`- 35 In addition to the above mentioned sorfactants, other suit2ble ~ surfactants can be found in the disclosure of U.S. Patents 3,544,473, r~ ' 3,63û,923, 3,8~8,781 and 4,0011132.
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~.:. * Trademark i . * * Trademark ' ' ,- .
`:
;~
~ 3 3 2 3 Alkali Metal Salt Dispenser Cup Caking Inhibitor The compositions of the invention contain from about 2% to about 20Yo~ preferably from about 4% to about 15%, of a dispencer cup caking .` inhibitor selected from the group consis-ting of alkali metal chlorides and mixtures thereof.
,.. ~ Operative dispenser cup caking inhibitors are in the form of dry `;~ powders having a particle size such that at least about 80% passes through a 3S Tyler mesh screen. The dispenser cup caking inhibitor is : added during the process of the inventi,on after at least about 30~0, , lO preferably about 75%, and most pre~erably about 90%, oF the water or "~ aqueous sodium silicate agglomerating agent has been added to the . ~;.
particulate cnmponents comprising sodium tripolyph~sphate.
. An especially preferred material is sodium chloride having a par-ticle size such that at least 8û% passes through a 100 Tyler mesh `` 15 screen.
s Water The compositions of the invention are made by a process in which ,'~,',5',' either water or an aqueous sodium silicate solution is used as the agglomerating agent.
- 20 The finished compositions will contain water in the form of hydra-, ted salts, preferably from about 9% to about 12% by weight.
, Alkali Metal Dichlorocyanurate . Sodium or potassium dichlorocyanurate is optionally but preferably ~, incorporated in the compositions of the invention in an am~unt suffi-, ,~ 25 cient to provide available chlorine equal to from about 0.75% to aboùt ,` 2.5% by weight of the composition. A preferred material is sodium dichlorocyanurate dihYdrate as disclosed in U~S. Patent 3~936~386 which provides 56% available chlorine by weight. The ability of a compound to provide hypochlorite ';;! 30 ion in solution is generally measured as "available chlorine". The . . .
, available chlorine reflects the m_thod of producing an inorganic hypo-; chlorite (e.g., 2 NaOH ~ C12 ~ NaOC1 ~ NaCl -~ H20). Avail-able chlorine is the chlorine liberated by acidification of a solution , , of hypochlorite ions and at least a molar equivalent amount of - , 35 chloride ions. The usual analytical method of determining available ,~ chlorine in a solution is addition of an excess of an iodide salt and ` titration of the liberated free iodine with a reducing agent.
:'. '^.~
, ~ ,.
:~l'733~3 ODtional Alkali ~etal Car~onates Optionally, the process and composition of the invention utilize alkali metal carbonate to provide the alkalinity needed ; for optimum cleaning performance.
Alkali metal carbonates, particularly sodium carbonate, can be present in the compositions at levels up to about 25% prefer-ably from about 2% to about 12% by weight.
Other Optional ~ngredients In addition to the above ingredients it can be desirable, - : 10 if the product sudses too much, to incorporate one of the many suds-suppressing ingredients disclosed in the above mentioned patents at a level of from about 0.01% to about 10%, preferably from about 0.05% to about 3%. The preferred suds suppressing - .
` materials are mono- and distearyl acid phosphates; the self-, 15 emuIsified siloxane suds suppressors of U.S. Patent 4,126,045 ~;~. and mixtures thereof.
~` Organic se~uestering builders such as citrates and nitrilotriacetates can be present in the compositions, but preferably at levels no greater than about 10% by weight. The ~; 20 presence of organic builders tends to hurt the performance of ~i these compositions by leaving visible spots and filming on 1'` ~
s~ glassware.
China protecting agents including aluminosilicates, aluminates, ~, etc., can be present in amounts up to about 5%, preferably from about 0.2% to about 2%.
~ Filler materials, sodium sulfate in particular, to control s ; product density and other physical characteristics can also be ~: present in amounts up to about 60%, preferably not more than about 30~ by weight.
Dyes, perfumes, crystal modifiers and the like can also be added in rninor amounts.
As used herein, all percentages, parts and ratios are by ;; weight unless otherwise stated.
r' ~ The following Examples illustrate the invention and facilitate ` 35 facilitate its understanding :
:
.
' ~
~ .
`~.; . ~173323 ' :
....
EXAMPLE I
A. 33.1 Parts by weight of powdered anhydrous sodium tripolyphosphate and 8.0 parts by weight of hydrous sodium silicate (82~ solids, SiO2:Na20 weight ratio of 2.4) were added to a ribbon mixer. With - - 5 the mixer in operation the following ingredients were added during a `~' cycle time of 180 seconds.
., a) from 0 seconds to ~65 seconds--added as a spray ~ blend of 1~.8 parts of an aqueous sodium silicate solution ,~; containing 47.3% silica-te solids with a Si~2:Na20 weight ratio of 2.0 and 4.7 parts of an aqueous sodium silicate solution containing 37.5% silicate solids with a ,~;, SiO2:Na20 weight ratio of 3.2. This solution also con-tained minor amounts of perfume and clye.
-~ b) at 60 seconds--added dry 19.4 parts of sodium sulfate and 10.0 parts of sodium car-~` bonate.
c) from 60 seconds to 165 seconds--added as a spray 4.0 parts of a polyoxyalkylene nonionic surfactant (condensa-y ' .
tion product of C18 alcohol with average of 8.25 moles ~; 20 ethylene oxide).
d) at 145 seconds--added dry 5cO parts of sodium chloride h~ving a particle size such that at least 80~ passed through a lûO Tyler mesh screen.
e) after 180 seconds -,~ 25 Product is discharged from mixer.
f) 2.5 parts of sodium dichlorocyanurate dihydrate was added and ; mixed in after drying and aging of the product discharged from the mixer at step e).
B. The process of A was repeated with the elimination of step d).
24.4 Parts sodium sulfate added at step b) replaced the.sodium chlor-ide of step d).
~ The compositions were packed in airtight containers pending evalu-; ~ ation. Resistance to automatic dishwasher dispenser cup caking was ; measured as indicated in the table below.
''' ,' .~. -~ ' .
~ ~3323 :. :
-- 10 -- .
Dispenser Cup Caking Grade Compnsition A B
- Automa-tic Dishwasher "Hotpoint'l ( trademark) end of main wash 0.6 3.0 middle of rinse 0.1 1.1 end of rinse 0.0 0.5 " Frigidaire" ( trademark) end of main wash 0.1 2.8 middle of rinse 0.0 1.6 end of rinse 0.0 0.6 - . ... ~ 1 ~ scale of 0-8. 0 indicating complete removal of product ,~ ;from cup, 8 indicating cup full of product.
Composition A was superior to Composition B in resistance to dis-:15 penser cup caking. No Composition A remained in the dispenser cup at the end of the rinse cycle, the point of principal notice of dispenser cup caking.
EXAMPLE II
The process of Example I-A was repeated with the substitution of NaCl having a particle size such that 80% passed through a 35 Tyler -mesh screen and less than 20% passed through a 10~ Tyler mesh screen.
The resultant composition was superior to Composition B sf Example I
but slightly inferior to Composition A of Example I.
EXAMPLE III
,~ 25 The materials listed in the~table below were added to Composition ,~ B of Example I at the levels and process cycle time indicated. 30û
grams of each resultant composition was mixed with 100 grams of 100F distilled water and stirred in a 400 ml beaker. Viscosity of the product slurries was measured by a Brookfield spindle viscometer !' 30 (#4 spindle/6 rpm) after seven minutes.
The reduction in viscosity for each additive was found to be pre-dictive of the improvement in resistance to dispenser cup caking.
, .
, .
. ., ~, .
. . .
~' .
~;` \\
- Dispenser Cup Caking Inhibitnr Viscosity (cps) None 28,000 1% NaCl--added at 165 sec. 22,500 2% NaCl--added at 165 sec. 14,000
5% NaCl--added at 165 sec. 6,000 : 10% NaCl--added at 165 sec. 1,400 , ~ ~ 10% NaCl--added at 60 sec. 2,700 .
3% NaCl (granular)--after end of cycle 25,000 : -i 4% NaCl (granular)--after end of cycle 8,000 ; 10 I0% NaCl (granular)--after end of cycle 4,800 ;' .
, 1% LiCl--added at 165 sec. 15,000 3% KCl--added at 165 sec. 16,000 10~ Li2S04--added at 165 sec. 15,000 10% Na3P04--added at 165 sec. 81000 15 9% Na2S04--added at 165 sec. ~ 28,000 9% Na2C03--added at 165 sec. ~28,000 9% sodium citrate--added at 165 sec. 12,500 3% sodium acetate--added at 165 sec. 18,000 All dispenser cup caking inhibitor materials listed above had a 20 particle size such that at least 80% by weight passed through a 100 Tyler mesh screen except granular NaCl for which 8~ passes through a ~, 35 Tyler mesh screen and 50% is retained on a 65 Tyler mesh screen.
WHAT IS CLAIME0 IS:
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3% NaCl (granular)--after end of cycle 25,000 : -i 4% NaCl (granular)--after end of cycle 8,000 ; 10 I0% NaCl (granular)--after end of cycle 4,800 ;' .
, 1% LiCl--added at 165 sec. 15,000 3% KCl--added at 165 sec. 16,000 10~ Li2S04--added at 165 sec. 15,000 10% Na3P04--added at 165 sec. 81000 15 9% Na2S04--added at 165 sec. ~ 28,000 9% Na2C03--added at 165 sec. ~28,000 9% sodium citrate--added at 165 sec. 12,500 3% sodium acetate--added at 165 sec. 18,000 All dispenser cup caking inhibitor materials listed above had a 20 particle size such that at least 80% by weight passed through a 100 Tyler mesh screen except granular NaCl for which 8~ passes through a ~, 35 Tyler mesh screen and 50% is retained on a 65 Tyler mesh screen.
WHAT IS CLAIME0 IS:
.,~;,; .
~,:
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Claims (7)
1. An agglomerated granular detergent composition consisting essentially of from about 15% to about 50% of sodium tripolyphosphate, from about 5% to about 25% silicate solids wherein the average SiO2:M2O weight ratio is from about 1.0 to about 3,6, M being an alkali metal, from about 2% to about 12% of a low-foaming nonionic surfactant selected from the group consisting of (a) the condensation product of 1 mole of a saturated or unsaturated, straight or branched chain, alcohol or fatty acid containing from about 10 to about 20 carbon atoms with from about 4 to about 50 moles of ethylene oxide;
(b) polyethylene glycols having molecular weights of from about 1,400 to about 30,000;
(c) the condensation products of 1 mole of alkyl phenol wherein the alkyl chain contains from about 8 to about 18 carbon atoms and from about 4 to about 50 moles of ethylene oxide;
(d) polyoxypropylene, polyoxyethylene condensates having the formula HO(C2H4O)x(C3H6O)y(C2H4O)xH
where y equals at least 15 and (C2H4O)x+x equals 20% to 90% of the total weight of the compound and the molecular weight is from about 2,000 to about 10,000;
(e) the compounds of (d) which are capped with propylene oxide, butylene oxide, alcohols or fatty acids, containing from 1 to about 5 carbon atoms;
(f) condensation products of ethylene oxide and propylene oxide with a low molecular weight trifunctional alcohol; and (g) mixtures thereof, and from about 2% to about 20% of a dispenser cup caking inhibitor selected from the group consisting of alkali metal chlorides selected from the group consisting of sodium chloride, potassium chloride, lithium chloride and mixtures thereof, said dispenser cup caking inhibitor being a dry material having a particle size such that at least about 80% passes through a 35 Tyler mesh screen, said agglome-rated granular detergent composition produced by agitating particulate components comprising anhydrous sodium tripolyphosphate, contacting said particulate components during said agitating with an agglomerating agent comprising water, mixing said agglomerating agent with said particulate components by continuing said agitating, adding said dispenser cup caking inhibitor during said agitating after at least about 30% of said agglomerating agent has been added to said particu-late components and recovering said agglomerated granular detergent composition.
(b) polyethylene glycols having molecular weights of from about 1,400 to about 30,000;
(c) the condensation products of 1 mole of alkyl phenol wherein the alkyl chain contains from about 8 to about 18 carbon atoms and from about 4 to about 50 moles of ethylene oxide;
(d) polyoxypropylene, polyoxyethylene condensates having the formula HO(C2H4O)x(C3H6O)y(C2H4O)xH
where y equals at least 15 and (C2H4O)x+x equals 20% to 90% of the total weight of the compound and the molecular weight is from about 2,000 to about 10,000;
(e) the compounds of (d) which are capped with propylene oxide, butylene oxide, alcohols or fatty acids, containing from 1 to about 5 carbon atoms;
(f) condensation products of ethylene oxide and propylene oxide with a low molecular weight trifunctional alcohol; and (g) mixtures thereof, and from about 2% to about 20% of a dispenser cup caking inhibitor selected from the group consisting of alkali metal chlorides selected from the group consisting of sodium chloride, potassium chloride, lithium chloride and mixtures thereof, said dispenser cup caking inhibitor being a dry material having a particle size such that at least about 80% passes through a 35 Tyler mesh screen, said agglome-rated granular detergent composition produced by agitating particulate components comprising anhydrous sodium tripolyphosphate, contacting said particulate components during said agitating with an agglomerating agent comprising water, mixing said agglomerating agent with said particulate components by continuing said agitating, adding said dispenser cup caking inhibitor during said agitating after at least about 30% of said agglomerating agent has been added to said particu-late components and recovering said agglomerated granular detergent composition.
2. The composition of Claim l wherein the dispenser cup caking inhibitor is sodium chloride.
3. The composition of Claim 2 wherein the dispenser cup caking inhibitor has a particle size such that at least 80%
passes through a 100 Tyler mesh screen.
passes through a 100 Tyler mesh screen.
4. The composition of Claims l, 2 or 3 wherein the dispenser cup caking inhibitor is added after at least about 75% of said agglomerating agent has been added to said particulate components.
5. The composition of Claims l, 2 or 3 which additionally includes an alkali metal dichlorocyanurate selected from the group consisting of sodium dichlorocyanurate, potassium dichlorocyanurate, and mixtures thereof, to provide an available chlorine level of from about 0.5% to about 3.0%.
6. The composition of Claims l, 2 or 3 wherein the low-foaming non-ionic surfactant consists essentially of a condensation product of an alcohol or a fatty acid containing from about 10 to about 20 carbon atoms with from about 4 to about 50 moles ethylene oxide.
7. The composition of Claims l, 2 or 3 wherein the low-foaming non-ionic surfactant consists essentially of a compound having the formula RO-(C2H4O)xR1 wherein R
is an alkyl or alkylene group containing from 17 to 19 carbon atoms, x is a number from about 6 to about 15 and R1 is selected from the group consisting of hydrogen, C1-5 alkyl groups, C2-5 acyl groups, groups having the formula -(CyH2yO)nH wherein y is 3 to 4 and n is from 1 to about 4.
is an alkyl or alkylene group containing from 17 to 19 carbon atoms, x is a number from about 6 to about 15 and R1 is selected from the group consisting of hydrogen, C1-5 alkyl groups, C2-5 acyl groups, groups having the formula -(CyH2yO)nH wherein y is 3 to 4 and n is from 1 to about 4.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US24328181A | 1981-03-13 | 1981-03-13 | |
| US243,281 | 1981-03-13 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1173323A true CA1173323A (en) | 1984-08-28 |
Family
ID=22918109
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000398237A Expired CA1173323A (en) | 1981-03-13 | 1982-03-12 | Agglomeration process for making granular detergents |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP0060587B1 (en) |
| CA (1) | CA1173323A (en) |
| DE (1) | DE3271854D1 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19801085A1 (en) * | 1998-01-14 | 1999-07-15 | Henkel Kgaa | Homogeneous surfactant granulate useful for making tablets e.g. toilet blocks |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4169806A (en) * | 1978-08-09 | 1979-10-02 | The Procter & Gamble Company | Agglomeration process for making granular detergents |
| DE2925137A1 (en) * | 1979-06-22 | 1981-01-08 | Keri Dipl Ing Karoly | Granular detergent compsns. - contg. specified amts. of tri:poly:phosphate, water and other ingredients |
-
1982
- 1982-03-01 DE DE8282200251T patent/DE3271854D1/en not_active Expired
- 1982-03-01 EP EP19820200251 patent/EP0060587B1/en not_active Expired
- 1982-03-12 CA CA000398237A patent/CA1173323A/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| DE3271854D1 (en) | 1986-08-07 |
| EP0060587A3 (en) | 1983-06-29 |
| EP0060587A2 (en) | 1982-09-22 |
| EP0060587B1 (en) | 1986-07-02 |
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