CA2259535C - Process for making detergent compositions - Google Patents
Process for making detergent compositions Download PDFInfo
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- CA2259535C CA2259535C CA002259535A CA2259535A CA2259535C CA 2259535 C CA2259535 C CA 2259535C CA 002259535 A CA002259535 A CA 002259535A CA 2259535 A CA2259535 A CA 2259535A CA 2259535 C CA2259535 C CA 2259535C
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- Prior art keywords
- surfactant
- particle size
- premix
- nonionic surfactant
- micrometers
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 230000008569 process Effects 0.000 title claims abstract description 23
- 239000000203 mixture Substances 0.000 title claims description 17
- 239000003599 detergent Substances 0.000 title claims description 14
- 239000002245 particle Substances 0.000 claims abstract description 73
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 36
- 239000000654 additive Substances 0.000 claims abstract description 24
- 239000004094 surface-active agent Substances 0.000 claims abstract description 18
- 239000003945 anionic surfactant Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 238000005507 spraying Methods 0.000 claims abstract description 6
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 34
- 239000011236 particulate material Substances 0.000 claims description 13
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 11
- 238000009826 distribution Methods 0.000 claims description 5
- MWNQXXOSWHCCOZ-UHFFFAOYSA-L sodium;oxido carbonate Chemical compound [Na+].[O-]OC([O-])=O MWNQXXOSWHCCOZ-UHFFFAOYSA-L 0.000 claims description 4
- 239000007844 bleaching agent Substances 0.000 claims description 2
- 239000010457 zeolite Substances 0.000 description 28
- 229910021536 Zeolite Inorganic materials 0.000 description 25
- -1 fatty acid esters Chemical class 0.000 description 21
- 239000000047 product Substances 0.000 description 15
- 235000014113 dietary fatty acids Nutrition 0.000 description 13
- 239000000194 fatty acid Substances 0.000 description 13
- 229930195729 fatty acid Natural products 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical group [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 9
- 150000004665 fatty acids Chemical class 0.000 description 9
- 238000005342 ion exchange Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 239000007921 spray Substances 0.000 description 8
- 125000000217 alkyl group Chemical group 0.000 description 7
- 229910021653 sulphate ion Inorganic materials 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerol Natural products OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 150000004996 alkyl benzenes Chemical class 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 5
- 239000007859 condensation product Substances 0.000 description 5
- 239000012530 fluid Substances 0.000 description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 4
- 229910001424 calcium ion Inorganic materials 0.000 description 4
- 125000004432 carbon atom Chemical group C* 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- 239000003760 tallow Substances 0.000 description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 230000009435 amidation Effects 0.000 description 2
- 238000007112 amidation reaction Methods 0.000 description 2
- 239000002518 antifoaming agent Substances 0.000 description 2
- 239000013522 chelant Substances 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- YGUMVDWOQQJBGA-VAWYXSNFSA-N 5-[(4-anilino-6-morpholin-4-yl-1,3,5-triazin-2-yl)amino]-2-[(e)-2-[4-[(4-anilino-6-morpholin-4-yl-1,3,5-triazin-2-yl)amino]-2-sulfophenyl]ethenyl]benzenesulfonic acid Chemical group C=1C=C(\C=C\C=2C(=CC(NC=3N=C(N=C(NC=4C=CC=CC=4)N=3)N3CCOCC3)=CC=2)S(O)(=O)=O)C(S(=O)(=O)O)=CC=1NC(N=C(N=1)N2CCOCC2)=NC=1NC1=CC=CC=C1 YGUMVDWOQQJBGA-VAWYXSNFSA-N 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical group OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 1
- MBBZMMPHUWSWHV-BDVNFPICSA-N N-methylglucamine Chemical compound CNC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO MBBZMMPHUWSWHV-BDVNFPICSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- ZUBJEHHGZYTRPH-KTKRTIGZSA-N [(z)-octadec-9-enyl] hydrogen sulfate Chemical compound CCCCCCCC\C=C/CCCCCCCCOS(O)(=O)=O ZUBJEHHGZYTRPH-KTKRTIGZSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 150000008051 alkyl sulfates Chemical class 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- UZABCLFSICXBCM-UHFFFAOYSA-N ethoxy hydrogen sulfate Chemical class CCOOS(O)(=O)=O UZABCLFSICXBCM-UHFFFAOYSA-N 0.000 description 1
- 235000019387 fatty acid methyl ester Nutrition 0.000 description 1
- 150000002193 fatty amides Chemical class 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 150000002314 glycerols Chemical class 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- CQDGTJPVBWZJAZ-UHFFFAOYSA-N monoethyl carbonate Chemical class CCOC(O)=O CQDGTJPVBWZJAZ-UHFFFAOYSA-N 0.000 description 1
- 235000014366 other mixer Nutrition 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229940071089 sarcosinate Drugs 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
- C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
- C11D11/0088—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads the liquefied ingredients being sprayed or adsorbed onto solid particles
Landscapes
- 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)
- Detergent Compositions (AREA)
Abstract
The present invention relates to a process comprising the steps of: (i) mixing together at least two non-surfactant additives to form a premix; (ii) spraying substantially all of the nonionic surfactant on to the premix to form a first intermediate particle; (iii) subsequently mixing the first intermediate particle with a second intermediate particle, wherein the second intermediate particle comprises substantially all of the anionic surfactant, and is substantially free of nonionic surfactant.
Description
PROCESS FOR MAKING DE7.'ERGENT COMPOSITIONS
The present invention relates to a process for making detergent compositions There is a trend amongst commercially available granular detergents towards higher bulk densities. This gives benefits both for consumer convenience and for reduction of packaging materials.
Many of the prior art attempts to move in this direction have met with problems of poor solubility properties arising from low rate of dissolution or the formation of gels. A consequence of this in a typical washing process can be poor dispensing of the product, either from the dispensing drawer of a washing machine, or from a dosing device placed with the laundry inside the machine. This poor dispensing is often caused by gelling of particles which have high levels of surfactant upon contact with water. The gel prevents a proportion of the detergent powder from being solubilised in the wash water which reduces the effectiveness of the powder. Another adverse consequence arises even if the ;powder is well dispensed and dispersed in the washing water if it does not dissolve rapidly. The wash cycle has a limited duration during which the detergent can act upon the laundry. If the cleaning action is delayed :because the powder is slow to dissolve, this, too, will limit the effectiveness of the powder.
The process engineer and formulator have frequently found that the need for good dispensing and the need for good dissolution rate have placed conflicting demands upon them. The solution has generally been to find a compromise which gives adequate dispensing and adequate dissolution rate. For example, poor dispensing of high bulk density granular detergents is often associated with surfactant rich particles having a high specific surface area, either due to high porosity or a small particle size (especially "fines"). However " decreasing the porosity and/or increasing the average particle size cause the dissolution rate to decrease.
W094/05761, published on 17th March 1994, describes a final product densification step wherein substantially all of the product is sprayed with nonionic surfactant and coated with zeolite. Good dispensing and dissolving properties are claimed.
However it has now been found that even further improvements in dispensing and dissolving properties can be achieved if the nonionic surfactant and zeolite coating is applied only to selected parts of the detergent composition, rather than to the detergent composition as a whole.
The object of the invention is to provide an improved process for making a detergent composition comprising anionic surfactant, nonionic surfactant and non-surfactant additives.
Summary of the Invention The object of the present invention is achieved by a process for making a detergent composition comprising anionic surfactant, nonionic surfactant and non-surfactant additives, the process comprising the steps of:
(i) mixing together at least two non--surfactant additives to form a premix;
(ii) spraying all of the nonionic surfactant on to the premix; subsequently applying a finely divided particulate material to the premix to form a first intermediate particle; and (iii) subsequently mixing the first intermediate particle with a second intermediate spray-dried or agglomerated particle, wherein the second intermediate spray-dried or agglomerated particle comprises from 20 to 40% by weight of anionic surfactant, and is free of nonionic surfactant.
Detailed Description of the Invention In a preferred embodiment of the process the first intermediate particle is formed by:
(a) mixing together at least two non-surfactant additives to form a premix; and (b) increasing the mean particle size of the premix by spraying nonionic surfactant on to the premix arid applying a finely divided particulate material, preferably aluminosilicate.
In a still further preferred embodiment of the process the first intermediate particle is formed by:
(a) mixing together at :least two non-surfactant additives to form a premix;
(b) spraying nonionic surfactant on to the premix wherein the ratio of nonionic surfactant to premix is at least 1:25;
(c) applying a first arnount of finely divided particulate material, wherein the ratio of the first amount of finely divided particulate material to nonionic surfactant applied in step (b) is less than 1:1;
The present invention relates to a process for making detergent compositions There is a trend amongst commercially available granular detergents towards higher bulk densities. This gives benefits both for consumer convenience and for reduction of packaging materials.
Many of the prior art attempts to move in this direction have met with problems of poor solubility properties arising from low rate of dissolution or the formation of gels. A consequence of this in a typical washing process can be poor dispensing of the product, either from the dispensing drawer of a washing machine, or from a dosing device placed with the laundry inside the machine. This poor dispensing is often caused by gelling of particles which have high levels of surfactant upon contact with water. The gel prevents a proportion of the detergent powder from being solubilised in the wash water which reduces the effectiveness of the powder. Another adverse consequence arises even if the ;powder is well dispensed and dispersed in the washing water if it does not dissolve rapidly. The wash cycle has a limited duration during which the detergent can act upon the laundry. If the cleaning action is delayed :because the powder is slow to dissolve, this, too, will limit the effectiveness of the powder.
The process engineer and formulator have frequently found that the need for good dispensing and the need for good dissolution rate have placed conflicting demands upon them. The solution has generally been to find a compromise which gives adequate dispensing and adequate dissolution rate. For example, poor dispensing of high bulk density granular detergents is often associated with surfactant rich particles having a high specific surface area, either due to high porosity or a small particle size (especially "fines"). However " decreasing the porosity and/or increasing the average particle size cause the dissolution rate to decrease.
W094/05761, published on 17th March 1994, describes a final product densification step wherein substantially all of the product is sprayed with nonionic surfactant and coated with zeolite. Good dispensing and dissolving properties are claimed.
However it has now been found that even further improvements in dispensing and dissolving properties can be achieved if the nonionic surfactant and zeolite coating is applied only to selected parts of the detergent composition, rather than to the detergent composition as a whole.
The object of the invention is to provide an improved process for making a detergent composition comprising anionic surfactant, nonionic surfactant and non-surfactant additives.
Summary of the Invention The object of the present invention is achieved by a process for making a detergent composition comprising anionic surfactant, nonionic surfactant and non-surfactant additives, the process comprising the steps of:
(i) mixing together at least two non--surfactant additives to form a premix;
(ii) spraying all of the nonionic surfactant on to the premix; subsequently applying a finely divided particulate material to the premix to form a first intermediate particle; and (iii) subsequently mixing the first intermediate particle with a second intermediate spray-dried or agglomerated particle, wherein the second intermediate spray-dried or agglomerated particle comprises from 20 to 40% by weight of anionic surfactant, and is free of nonionic surfactant.
Detailed Description of the Invention In a preferred embodiment of the process the first intermediate particle is formed by:
(a) mixing together at least two non-surfactant additives to form a premix; and (b) increasing the mean particle size of the premix by spraying nonionic surfactant on to the premix arid applying a finely divided particulate material, preferably aluminosilicate.
In a still further preferred embodiment of the process the first intermediate particle is formed by:
(a) mixing together at :least two non-surfactant additives to form a premix;
(b) spraying nonionic surfactant on to the premix wherein the ratio of nonionic surfactant to premix is at least 1:25;
(c) applying a first arnount of finely divided particulate material, wherein the ratio of the first amount of finely divided particulate material to nonionic surfactant applied in step (b) is less than 1:1;
4 _ (d) increasing the mean particle size of the premix by mixing; and (e) applying a second amount of finely divided particulate material, wherein the second amount of finely divided particulate material to nonionic surfactant applied in step (b) is greater than 1:1.
The process of the invention results in a narrow particle size distribution with a sharply defined mean. Preferably the mean particle size is 800 to 1200 micrometers, and the particle size distribution has a standard deviation of less than 100 micrometers. More preferably the mean particle size is from 900 to 1100 micrometers, and the particle size distribution has a standard deviation of less than 50 micrometers.
Non-surfactant additives may include any detergent additives such as bleach, especially perborate or percarbonate; inorganic salts, especially carbonate, bicarbonate, silicate, sulphate, or citrate; chelants, enzymes.
Preferably the first intermediate particle comprises less than 5% by weight of anionic surfactant, more preferably the first intermediate particle comprises less than 1% by weight of anionic surfactant.
Finely divided particulate materials useful herein include aluminosilicates having the empirical formula:
Mz ( zA102 ) y ] ~ x H20 wherein z and y are integers of at least 6, the molar ratio of z to y is in the range from 1.0 to about 0.5, and x is an integer from about 15 to about 264.
-Useful aluminosilicate ion exchange materials are commercially available. These a.luminosilicates can be crystalline or amorphous in structure and can be naturally-occurring aluminosilicates or synthetically derived. A
method for producing aluminosilicate ion exchange materials is disclosed in US-A-3 985 669, Krummel et al, issued October 12, 1976. Preferred synthetic crystalline aluminosilicate ion exchange materials useful herein are available under the designations zeolite A, zeolite P(B), zeolite MAP, zeolite X and zeolite Y. In an especially preferred embodiment, the crystalline aluminosilicate ion exchange material has the formula .
Nal2 [ (A102) 12 (SiO2) 12 l ~ x H20 wherein x is from about 20 to about 30, especially about 27. This material is known as zeolite A. Dehydrated zeolites (x=0-10), and "overdried" zeolites (x=10-20) may also be used herein. The "overdried" zeolites are particularly useful when a low moisture environment is required, for example to improve stability of detergent bleaches such as perborate and percarbonate. Preferably, the aluminosilicate has a particle size of about 0.1-10 micrometers in diameter. Preferred ion exchange materials have a particle size diameter of from about 0.2 micrometers to about 4 micrometers. The term "particle size diameter"
herein represents the average particle size diameter by weight of a given ion exchange material as determined by conventional analytical techniques such as, for example, microscopic determination utilizing a scanning electron microscope. The crystalline zeolite A materials herein are usually further characterized by their calcium ion exchange capacity, which is at least abovut 200 mg equivalent of CaC03 water hardness/g of alumi:nosilicate, calculated on an anhydrous basis, and which generally is in the range of from about 300 mg eq./g to about 352 mg eq./g. The zeolite 6 _ A materials herein are still further characterized by their calcium ion exchange rate which is at least about 2 grains Ca++/gallon/minute/gram/gallon (0.138 Ca++/litre/minute/gram/litre) of aluminosilicate (anhydrous basis), and generally lies within the range of from about 2 grains/gallon/minute/gram/gallon(0.13g Ca++/litre/minute/gram/litre) to about 6 grains/gallon/minute/gram/gallon (0.398 Ca++/litre/minute/gram/litre), based on calcium ion hardness. Optimum aluminosilicate for builder purposes exhibit a calcium ion exchange rate of at least about 4 grains/gallon/minute/gram/gallon (0.26g Ca++/litre/minute/gram/litre).
While any nonionic surfactant may be usefully employed in the present invention, two families of nonionics have been found to be particularly useful. These are nonionic surfactants based on alkoxylated (especially ethoxylated) alcohols, and those nonionic surfactants based on amidation products of fatty acid esters and N-alkyl polyhydroxy amine. The amidation products of the esters and the amines are generally referred to herein as polyhydroxy fatty acid amides. Particularly useful in the present invention are mixtures comprising two or more nonionic surfactants wherein at least one nonionic surfactant is selected from each of the groups of alkoxylated alcohols and the polyhydroxy fatty acid amides.
Suitable nonionic surfactants include compounds produced by the condensation of alkylene oxide groups (hydrophilic in nature) with an organic hydrophobic compound, which may be aliphatic or alkyl aromatic in nature. The length of the polyoxyalkylene group which is condensed with any particular hydrophobic group can be readily adjusted to yield a water-soluble compound having the desired degree of balance between hydrophilic and hydrophobic elements.
Particularly preferred for use in the present invention are nonionic surfactants such as the polyethylene oxide condensates of alkyl phenols, e.g., the condensation products of alkyl phenols having an alkyl group containing from about 6 to 16 carbon atoms, in either a straight chain or branched chain configuration, with from about 4 to 25 moles of ethylene oxide per mole of alkyl phenol.
Preferred nonionics are the water-soluble condensation products of aliphatic alcohols containing from 8 to 22 carbon atoms, in either straight chain or branched configuration, with an average of up to 25 moles of ethylene oxide per more of alcohol. Particularly preferred are the condensation products of alcohols having an alkyl group containing from about 9 to 15 carbon atoms with from about 2 to 10 moles of ethylene oxide per mole of alcohol;
and condensation products of propylene glycol with ethylene oxide. Most preferred are condensation products of alcohols having an alkyl group containing from about 12 to 15 carbon atoms with an average of about 3 moles of ethylene oxide per mole of alcohol.
It is a particularly preferred embodiment of the present invention that the nonionic surfactant system also includes a polyhydroxy fatty acid amide component.
Polyhydroxy fatty acid amides may be produced by reacting a fatty acid ester and an N-alkyl polyhydroxy amine. The preferred amine for use in the present invention is N-(R1)-CHz (CH20H) 4-CHZ-OH, where Rl is typically alkyl, e.g.
methyl group; and the preferred ester is a C12-C20 fatty acid methyl ester.
Methods of manufacturing polyhydroxy fatty acid amides have been described in WO 92 6073, published on 16th April, 1992. This application describes the preparation of polyhydroxy fatty acid amides in the presence of solvents.
In a highly preferred embodiment of the invention N-methyl glucamine is reacted with a C12-C20 methyl ester.
Other nonionic surfactants which may be used as components of the surfactant systems herein include ethoxylated nonionic surfactants, glycerol ethers, glucosamides, glycerol amides, glycerol esters, fatty acids, fatty acid esters, fatty amides, alkyl polyglucosides, alkyl polyglycol ethers, polyethylene glycols, ethoxylated alkyl phenols and mixtures thereof.
The second intermediate particle of the present invention comprises anionic surfactant. The second intermediate particle may be made by any process including spray drying, flaking, prilling, extruding, pastillating, and agglomeration. Agglomeration processes for making anionic surfactant particles have been disclosed in the prior art in, for example, EP-A-0 508 543, EP-A-0 510 746, EP-A-0 618 289 and EP-A-0 663 439. An essential feature of the invention is that no nonionic surfactant is sprayed on to the surfactant agglomerate stream.
Non-limiting examples of anionic surfactants useful herein include the conventional C11-C18 alkyl benzene sulfonates ("LAS") and primary, branched-chain and random C10-C20 alkyl sulfates ("AS"), the C10-C18 secondary (2,3) alkyl sulfates of the formula CH3 (CH2)x (CHOS03-M+) CH3 and CH3 (CH2)y(CHOS03-M+) CH2 CH3 where x and (y+1) are integers of at least about 7, preferably at least about 9, and M is a p water-solubilizing cation, especially sodium, unsaturated sulfates such as oleyl sulfate, the C10-C18 alkyl alkoxy sulfates ("AExS", especially EO 1-7 ethoxy sulfates), C10-C18 alkyl alkoxy carboxylates (especially the EO 1-5 ethoxycarboxylates), the C10-C18 glycerol ethers, the C10-C18 alkyl polyglycosides and their corresponding sulfated polyglycosides, the C12-C18 alpha-sulfonated fatty acid esters, methyl ester sulphonat~e and oleoyl sarcosinate.
Finally the surfactant agglomerates and layered granular additives are mixed, optionally with additional additives to form a finished detergent composition.
The various mixing steps of thcs present invention may be carried out in any suitable mixer such as the Eirich~, series RV, manufactured by Gust=au Eirich Hardheim, Germany;
Lodige°, series FM for batch mixing, series Baud KM for continuous mixing/agglomeration, manufactured by Lodige Machinenbau GmbH, Paderborn Ge~__~many; Drais~ T160 series, manufactured by Drais Werke GmbH, Mannheim Germany; and Winkworth° RT 25 series, manufactured by Winkworth Machinery Ltd., Berkshire, Eng:Land; the Littleford Mixer, Model #FM-130-D-12, with internal chopping blades and the Cuisinart Food Processor, Mode=L #DCX-Plus, with 7.75 inch (19.7 cm) blades. Many other mixers are commercially available for both batch and continuous mixing.
WO 98!01520 PCT/US97/11281 Examples Example Example Example Example Example Sodium carbonate 3 2 2 7.8 Sodium citrate - - - - 10 Sodium - - - - 10 bicarbonate Percarbonate 20 16 16 - -Perborate - - - 18 -Enzymes 1.7 2.2 2.2 1 2 Nonionic 4 13 19 20 20 surfactant particles Hydroxy ethylene 1 1 1 -diphosphonic acid Tetraacetyl 6 4.7 4.7 4 -ethylene diamine Antifoam particle 2.8 1 1 - -Layered silicate 15 12 12 - -Sodium silicate - - - 2 3 (2.0R) Sodium sulphate - - - - 5 Cationic 5 - - - -surfactant particles Brightener - - - 0.2 -58.5 51.9 57.9 53 50 All percentages expressed by weight of finis hed product are unless otherwise ated.
st Nonionic surfactantparticles contained 15 parts alcohol ethoxylate with average 5 EO grou ps per le, AE5,15 an of mo parts of polyhydroxy fatty 60 parts zeolite,5 acid amide, parts fatty acid and 5 parts water, and were made according to the process disclosed in EP-A-0 643 130.
Antifoam particles contained lc. parts silicone oil, 70 parts starch and 12 parts hydrogenated fatty acid / tallow alcohol ethoxylate (TAE80), anal were made according to the process disclosed in EP-A-0 495 345.
Layered silicate is SKS-6° supplied by Hoechst Cationic surfactant particles contained 30 parts alkyl dimethyl ethoxy ammonium chloride, 60 parts sodium sulphate, 5 parts alkyl sulphate and 5 parts water and were made according to the process disclosed in EP-A-0 714 976.
Brightener is Tinopal CDX° supplied by Ciba-Geigy.
Example 1 The additives shown under Example 1 in the previous table were mixed together and found to have an average particle size of 440 micrometers.
6.5% of nonionic surfactant (alcohol ethoxylate with an average of 5 EO groups per mole, AE5) at 35°C was sprayed onto the additive mixture in a concrete mixer using a two-fluid spray nozzle. 5% of zeolite A was added into the concrete mixer over a period of 1 minute. The mixer then continued to operate without further addition of zeolite for a further one and a half minutes. Finally a further 8%
of zeolite was added over a period of 1 minute.
The product in the concrete mixer had an average particle size of 1020 micrometers.
An anionic surfactant particle was then added to the concrete mixer at a level of 22%. The anionic surfactant particle contained 28 parts linear alkyl benzene sulphonate, 12 parts tallow alkyl sulphate, 30 parts zeolite, 20 parts carbonate and 10 parts water, and had an average particle size of 850 micrometers.
The finished product had an average particle size of 960 micrometers.
Example 2 The additives shown under Example 2 in the previous table were mixed together and found to have an average particle size of 390 micrometers.
6.5% of nonionic surfactant (AE5) at 35°C was sprayed onto the additive mixture in a concrete mixer using a two-fluid spray nozzle. 4% of zeolite A w,as added into the concrete mixer over a period of 1 minute. The mixer then continued to operate without further addition of zeolite for a further one minute. Finally a further 9% of zeolite was added over a period of 2 minutes.
The product in the concrete mixE_r had an average particle size of 1080 micrometers.
An anionic surfactant particle was then added to the concrete mixer at a level of 28.,6%. The anionic surfactant particle contained 28 parts linear alkyl benzene sulphonate, 12 parts tallow alkyl sulphate, 30 parts zeolite, 20 parts carbonate and 10 parts water, and had an average particle size of 850 micrometers.
The finished product had an average particle size of 1030 micrometers.
Example 3 The additives shown under Example 3 in the previous table were mixed together and found to have an average particle size of 390 micrometers.
6.5% of nonionic surfactant (AE5) at 35°C was sprayed onto the additive mixture in a concreae mixer using a two-fluid spray nozzle. 7% of zeolite A wa.s added into the concrete mixer in a single step.
The product in the concrete mixer had an average particle size of 555 micrometers.
An anionic surfactant particle was then added to the concrete mixer at a level of 28.60. The anionic surfactant particle contained 28 parts linear alkyl benzene sulphonate, 12 parts tallow alkyl sulphate, 30 parts zeolite, 20 parts carbonate and 10 parts water, and had an average particle size of 410 micrometers.
The finished product had an average particle size of 520 micrometers.
Example 4 The additives shown under Example 4 in the previous table were mixed together.
6% of nonionic surfactant (AE5) at 35°C was sprayed onto the additive mixture in a concrete mixer using a two-fluid spray nozzle. 13% of zeolite A were added into the concrete mixer in discrete portions, 1% at a time.
The product in the concrete mixer had an average particle size of 1000 micrometers.
A spray dried powder was then added to the concrete mixer at a level of 28%. The spray dried particle contained 20 parts linear alkyl benzene sulphonate, 5 parts polyacrylate polymer, 5 parts of chelant, 30 parts zeolite, 30 parts sulphate and 10 parts water, and had an average particle size of 1000 micrometers.
The finished product had an average particle size of 1000 micrometers.
1 ~~
Example 5 The additives shown under Example 5 in the previous table were mixed together.
7% of nonionic surfactant (AE5) at 35°C was sprayed onto the additive mixture in a concrete mixer using a two-fluid spray nozzle. 13% of zeolite A were added into the concrete mixer in discrete portions, 1% at a time.
The product in the concrete mixer had an average particle size of 1050 micrometers.
A spray-dried granule was then added to the concrete mixer at a level of 30%. The spray dried particle contained 20 parts linear alkyl benzene sulp.honate, 5 parts polyacrylate polymer, 5 parts of chelant, 30 parts zeolite, 30 parts sulphate and 10 parts water, and had an average particle size of 1000 micrometers.
The finished product had an average particle size of 1020 micrometers.
The process of the invention results in a narrow particle size distribution with a sharply defined mean. Preferably the mean particle size is 800 to 1200 micrometers, and the particle size distribution has a standard deviation of less than 100 micrometers. More preferably the mean particle size is from 900 to 1100 micrometers, and the particle size distribution has a standard deviation of less than 50 micrometers.
Non-surfactant additives may include any detergent additives such as bleach, especially perborate or percarbonate; inorganic salts, especially carbonate, bicarbonate, silicate, sulphate, or citrate; chelants, enzymes.
Preferably the first intermediate particle comprises less than 5% by weight of anionic surfactant, more preferably the first intermediate particle comprises less than 1% by weight of anionic surfactant.
Finely divided particulate materials useful herein include aluminosilicates having the empirical formula:
Mz ( zA102 ) y ] ~ x H20 wherein z and y are integers of at least 6, the molar ratio of z to y is in the range from 1.0 to about 0.5, and x is an integer from about 15 to about 264.
-Useful aluminosilicate ion exchange materials are commercially available. These a.luminosilicates can be crystalline or amorphous in structure and can be naturally-occurring aluminosilicates or synthetically derived. A
method for producing aluminosilicate ion exchange materials is disclosed in US-A-3 985 669, Krummel et al, issued October 12, 1976. Preferred synthetic crystalline aluminosilicate ion exchange materials useful herein are available under the designations zeolite A, zeolite P(B), zeolite MAP, zeolite X and zeolite Y. In an especially preferred embodiment, the crystalline aluminosilicate ion exchange material has the formula .
Nal2 [ (A102) 12 (SiO2) 12 l ~ x H20 wherein x is from about 20 to about 30, especially about 27. This material is known as zeolite A. Dehydrated zeolites (x=0-10), and "overdried" zeolites (x=10-20) may also be used herein. The "overdried" zeolites are particularly useful when a low moisture environment is required, for example to improve stability of detergent bleaches such as perborate and percarbonate. Preferably, the aluminosilicate has a particle size of about 0.1-10 micrometers in diameter. Preferred ion exchange materials have a particle size diameter of from about 0.2 micrometers to about 4 micrometers. The term "particle size diameter"
herein represents the average particle size diameter by weight of a given ion exchange material as determined by conventional analytical techniques such as, for example, microscopic determination utilizing a scanning electron microscope. The crystalline zeolite A materials herein are usually further characterized by their calcium ion exchange capacity, which is at least abovut 200 mg equivalent of CaC03 water hardness/g of alumi:nosilicate, calculated on an anhydrous basis, and which generally is in the range of from about 300 mg eq./g to about 352 mg eq./g. The zeolite 6 _ A materials herein are still further characterized by their calcium ion exchange rate which is at least about 2 grains Ca++/gallon/minute/gram/gallon (0.138 Ca++/litre/minute/gram/litre) of aluminosilicate (anhydrous basis), and generally lies within the range of from about 2 grains/gallon/minute/gram/gallon(0.13g Ca++/litre/minute/gram/litre) to about 6 grains/gallon/minute/gram/gallon (0.398 Ca++/litre/minute/gram/litre), based on calcium ion hardness. Optimum aluminosilicate for builder purposes exhibit a calcium ion exchange rate of at least about 4 grains/gallon/minute/gram/gallon (0.26g Ca++/litre/minute/gram/litre).
While any nonionic surfactant may be usefully employed in the present invention, two families of nonionics have been found to be particularly useful. These are nonionic surfactants based on alkoxylated (especially ethoxylated) alcohols, and those nonionic surfactants based on amidation products of fatty acid esters and N-alkyl polyhydroxy amine. The amidation products of the esters and the amines are generally referred to herein as polyhydroxy fatty acid amides. Particularly useful in the present invention are mixtures comprising two or more nonionic surfactants wherein at least one nonionic surfactant is selected from each of the groups of alkoxylated alcohols and the polyhydroxy fatty acid amides.
Suitable nonionic surfactants include compounds produced by the condensation of alkylene oxide groups (hydrophilic in nature) with an organic hydrophobic compound, which may be aliphatic or alkyl aromatic in nature. The length of the polyoxyalkylene group which is condensed with any particular hydrophobic group can be readily adjusted to yield a water-soluble compound having the desired degree of balance between hydrophilic and hydrophobic elements.
Particularly preferred for use in the present invention are nonionic surfactants such as the polyethylene oxide condensates of alkyl phenols, e.g., the condensation products of alkyl phenols having an alkyl group containing from about 6 to 16 carbon atoms, in either a straight chain or branched chain configuration, with from about 4 to 25 moles of ethylene oxide per mole of alkyl phenol.
Preferred nonionics are the water-soluble condensation products of aliphatic alcohols containing from 8 to 22 carbon atoms, in either straight chain or branched configuration, with an average of up to 25 moles of ethylene oxide per more of alcohol. Particularly preferred are the condensation products of alcohols having an alkyl group containing from about 9 to 15 carbon atoms with from about 2 to 10 moles of ethylene oxide per mole of alcohol;
and condensation products of propylene glycol with ethylene oxide. Most preferred are condensation products of alcohols having an alkyl group containing from about 12 to 15 carbon atoms with an average of about 3 moles of ethylene oxide per mole of alcohol.
It is a particularly preferred embodiment of the present invention that the nonionic surfactant system also includes a polyhydroxy fatty acid amide component.
Polyhydroxy fatty acid amides may be produced by reacting a fatty acid ester and an N-alkyl polyhydroxy amine. The preferred amine for use in the present invention is N-(R1)-CHz (CH20H) 4-CHZ-OH, where Rl is typically alkyl, e.g.
methyl group; and the preferred ester is a C12-C20 fatty acid methyl ester.
Methods of manufacturing polyhydroxy fatty acid amides have been described in WO 92 6073, published on 16th April, 1992. This application describes the preparation of polyhydroxy fatty acid amides in the presence of solvents.
In a highly preferred embodiment of the invention N-methyl glucamine is reacted with a C12-C20 methyl ester.
Other nonionic surfactants which may be used as components of the surfactant systems herein include ethoxylated nonionic surfactants, glycerol ethers, glucosamides, glycerol amides, glycerol esters, fatty acids, fatty acid esters, fatty amides, alkyl polyglucosides, alkyl polyglycol ethers, polyethylene glycols, ethoxylated alkyl phenols and mixtures thereof.
The second intermediate particle of the present invention comprises anionic surfactant. The second intermediate particle may be made by any process including spray drying, flaking, prilling, extruding, pastillating, and agglomeration. Agglomeration processes for making anionic surfactant particles have been disclosed in the prior art in, for example, EP-A-0 508 543, EP-A-0 510 746, EP-A-0 618 289 and EP-A-0 663 439. An essential feature of the invention is that no nonionic surfactant is sprayed on to the surfactant agglomerate stream.
Non-limiting examples of anionic surfactants useful herein include the conventional C11-C18 alkyl benzene sulfonates ("LAS") and primary, branched-chain and random C10-C20 alkyl sulfates ("AS"), the C10-C18 secondary (2,3) alkyl sulfates of the formula CH3 (CH2)x (CHOS03-M+) CH3 and CH3 (CH2)y(CHOS03-M+) CH2 CH3 where x and (y+1) are integers of at least about 7, preferably at least about 9, and M is a p water-solubilizing cation, especially sodium, unsaturated sulfates such as oleyl sulfate, the C10-C18 alkyl alkoxy sulfates ("AExS", especially EO 1-7 ethoxy sulfates), C10-C18 alkyl alkoxy carboxylates (especially the EO 1-5 ethoxycarboxylates), the C10-C18 glycerol ethers, the C10-C18 alkyl polyglycosides and their corresponding sulfated polyglycosides, the C12-C18 alpha-sulfonated fatty acid esters, methyl ester sulphonat~e and oleoyl sarcosinate.
Finally the surfactant agglomerates and layered granular additives are mixed, optionally with additional additives to form a finished detergent composition.
The various mixing steps of thcs present invention may be carried out in any suitable mixer such as the Eirich~, series RV, manufactured by Gust=au Eirich Hardheim, Germany;
Lodige°, series FM for batch mixing, series Baud KM for continuous mixing/agglomeration, manufactured by Lodige Machinenbau GmbH, Paderborn Ge~__~many; Drais~ T160 series, manufactured by Drais Werke GmbH, Mannheim Germany; and Winkworth° RT 25 series, manufactured by Winkworth Machinery Ltd., Berkshire, Eng:Land; the Littleford Mixer, Model #FM-130-D-12, with internal chopping blades and the Cuisinart Food Processor, Mode=L #DCX-Plus, with 7.75 inch (19.7 cm) blades. Many other mixers are commercially available for both batch and continuous mixing.
WO 98!01520 PCT/US97/11281 Examples Example Example Example Example Example Sodium carbonate 3 2 2 7.8 Sodium citrate - - - - 10 Sodium - - - - 10 bicarbonate Percarbonate 20 16 16 - -Perborate - - - 18 -Enzymes 1.7 2.2 2.2 1 2 Nonionic 4 13 19 20 20 surfactant particles Hydroxy ethylene 1 1 1 -diphosphonic acid Tetraacetyl 6 4.7 4.7 4 -ethylene diamine Antifoam particle 2.8 1 1 - -Layered silicate 15 12 12 - -Sodium silicate - - - 2 3 (2.0R) Sodium sulphate - - - - 5 Cationic 5 - - - -surfactant particles Brightener - - - 0.2 -58.5 51.9 57.9 53 50 All percentages expressed by weight of finis hed product are unless otherwise ated.
st Nonionic surfactantparticles contained 15 parts alcohol ethoxylate with average 5 EO grou ps per le, AE5,15 an of mo parts of polyhydroxy fatty 60 parts zeolite,5 acid amide, parts fatty acid and 5 parts water, and were made according to the process disclosed in EP-A-0 643 130.
Antifoam particles contained lc. parts silicone oil, 70 parts starch and 12 parts hydrogenated fatty acid / tallow alcohol ethoxylate (TAE80), anal were made according to the process disclosed in EP-A-0 495 345.
Layered silicate is SKS-6° supplied by Hoechst Cationic surfactant particles contained 30 parts alkyl dimethyl ethoxy ammonium chloride, 60 parts sodium sulphate, 5 parts alkyl sulphate and 5 parts water and were made according to the process disclosed in EP-A-0 714 976.
Brightener is Tinopal CDX° supplied by Ciba-Geigy.
Example 1 The additives shown under Example 1 in the previous table were mixed together and found to have an average particle size of 440 micrometers.
6.5% of nonionic surfactant (alcohol ethoxylate with an average of 5 EO groups per mole, AE5) at 35°C was sprayed onto the additive mixture in a concrete mixer using a two-fluid spray nozzle. 5% of zeolite A was added into the concrete mixer over a period of 1 minute. The mixer then continued to operate without further addition of zeolite for a further one and a half minutes. Finally a further 8%
of zeolite was added over a period of 1 minute.
The product in the concrete mixer had an average particle size of 1020 micrometers.
An anionic surfactant particle was then added to the concrete mixer at a level of 22%. The anionic surfactant particle contained 28 parts linear alkyl benzene sulphonate, 12 parts tallow alkyl sulphate, 30 parts zeolite, 20 parts carbonate and 10 parts water, and had an average particle size of 850 micrometers.
The finished product had an average particle size of 960 micrometers.
Example 2 The additives shown under Example 2 in the previous table were mixed together and found to have an average particle size of 390 micrometers.
6.5% of nonionic surfactant (AE5) at 35°C was sprayed onto the additive mixture in a concrete mixer using a two-fluid spray nozzle. 4% of zeolite A w,as added into the concrete mixer over a period of 1 minute. The mixer then continued to operate without further addition of zeolite for a further one minute. Finally a further 9% of zeolite was added over a period of 2 minutes.
The product in the concrete mixE_r had an average particle size of 1080 micrometers.
An anionic surfactant particle was then added to the concrete mixer at a level of 28.,6%. The anionic surfactant particle contained 28 parts linear alkyl benzene sulphonate, 12 parts tallow alkyl sulphate, 30 parts zeolite, 20 parts carbonate and 10 parts water, and had an average particle size of 850 micrometers.
The finished product had an average particle size of 1030 micrometers.
Example 3 The additives shown under Example 3 in the previous table were mixed together and found to have an average particle size of 390 micrometers.
6.5% of nonionic surfactant (AE5) at 35°C was sprayed onto the additive mixture in a concreae mixer using a two-fluid spray nozzle. 7% of zeolite A wa.s added into the concrete mixer in a single step.
The product in the concrete mixer had an average particle size of 555 micrometers.
An anionic surfactant particle was then added to the concrete mixer at a level of 28.60. The anionic surfactant particle contained 28 parts linear alkyl benzene sulphonate, 12 parts tallow alkyl sulphate, 30 parts zeolite, 20 parts carbonate and 10 parts water, and had an average particle size of 410 micrometers.
The finished product had an average particle size of 520 micrometers.
Example 4 The additives shown under Example 4 in the previous table were mixed together.
6% of nonionic surfactant (AE5) at 35°C was sprayed onto the additive mixture in a concrete mixer using a two-fluid spray nozzle. 13% of zeolite A were added into the concrete mixer in discrete portions, 1% at a time.
The product in the concrete mixer had an average particle size of 1000 micrometers.
A spray dried powder was then added to the concrete mixer at a level of 28%. The spray dried particle contained 20 parts linear alkyl benzene sulphonate, 5 parts polyacrylate polymer, 5 parts of chelant, 30 parts zeolite, 30 parts sulphate and 10 parts water, and had an average particle size of 1000 micrometers.
The finished product had an average particle size of 1000 micrometers.
1 ~~
Example 5 The additives shown under Example 5 in the previous table were mixed together.
7% of nonionic surfactant (AE5) at 35°C was sprayed onto the additive mixture in a concrete mixer using a two-fluid spray nozzle. 13% of zeolite A were added into the concrete mixer in discrete portions, 1% at a time.
The product in the concrete mixer had an average particle size of 1050 micrometers.
A spray-dried granule was then added to the concrete mixer at a level of 30%. The spray dried particle contained 20 parts linear alkyl benzene sulp.honate, 5 parts polyacrylate polymer, 5 parts of chelant, 30 parts zeolite, 30 parts sulphate and 10 parts water, and had an average particle size of 1000 micrometers.
The finished product had an average particle size of 1020 micrometers.
Claims (6)
1. A process for making a detergent composition comprising anionic surfactant, nonionic surfactant and non-surfactant additives, the process comprising the steps of:
(i) mixing together at least two non-surfactant additives to form a premix;
(ii) spraying all of the nonionic surfactant on to the premix; subsequently applying a finely divided particulate material to the premix to form a first intermediate particle; and (iii) subsequently mixing the first intermediate particle with a second intermediate spray-dried or agglomerated particle, wherein the second intermediate spray-dried or agglomerated particle comprises from 20 to 40% by weight of anionic surfactant, and is free of nonionic surfactant.
(i) mixing together at least two non-surfactant additives to form a premix;
(ii) spraying all of the nonionic surfactant on to the premix; subsequently applying a finely divided particulate material to the premix to form a first intermediate particle; and (iii) subsequently mixing the first intermediate particle with a second intermediate spray-dried or agglomerated particle, wherein the second intermediate spray-dried or agglomerated particle comprises from 20 to 40% by weight of anionic surfactant, and is free of nonionic surfactant.
2. A process according to claim 1 wherein the first intermediate particle is formed by:
(a) mixing together at least two non-surfactant additives to form a premix;
(b) spraying nonionic surfactant on to the premix wherein the ratio of nonionic surfactant to premix is at least 1:25;
(c) applying a first amount of finely divided particulate material, wherein the ratio of the first amount of finely divided particulate material to nonionic surfactant applied in step (b) is less than 1:1;
(d) increasing the mean particle size of the premix by mixing; and (e) applying a second amount of finely divided particulate material, wherein the second amount of finely divided particulate material to nonionic surfactant applied in step (b) is greater than 1:1.
(a) mixing together at least two non-surfactant additives to form a premix;
(b) spraying nonionic surfactant on to the premix wherein the ratio of nonionic surfactant to premix is at least 1:25;
(c) applying a first amount of finely divided particulate material, wherein the ratio of the first amount of finely divided particulate material to nonionic surfactant applied in step (b) is less than 1:1;
(d) increasing the mean particle size of the premix by mixing; and (e) applying a second amount of finely divided particulate material, wherein the second amount of finely divided particulate material to nonionic surfactant applied in step (b) is greater than 1:1.
3. A process according to claim 2 wherein the first intermediate particle has a mean particle size of from 800 to 1200 micrometers, and the particle size distribution has a standard deviation of less than 100 micrometers.
4. A process according to claim 3 wherein the first intermediate particle has a mean particle size of from 900 to 1100 micrometers, and the particle size distribution has a standard deviation of less than 50 micrometers.
5. A process according to claim 1 wherein the finely divided particulate material is aluminosilicate.
6. A process according to claim 1 wherein at least one of the non-surfactant additives is a bleach selected from the group consisting o~ perborate, percarbonate, and mixtures thereof.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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EP96201854.5 | 1996-07-04 | ||
EP96201854A EP0816485B1 (en) | 1996-07-04 | 1996-07-04 | Process for making detergent compositions |
PCT/US1997/011281 WO1998001520A2 (en) | 1996-07-04 | 1997-06-27 | Process for making detergent compositions |
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CA2259535A1 CA2259535A1 (en) | 1998-01-15 |
CA2259535C true CA2259535C (en) | 2002-10-01 |
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CA002259535A Expired - Fee Related CA2259535C (en) | 1996-07-04 | 1997-06-27 | Process for making detergent compositions |
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EP (1) | EP0816485B1 (en) |
JP (1) | JPH11514033A (en) |
CN (1) | CN1195834C (en) |
AR (1) | AR008062A1 (en) |
AT (1) | ATE312901T1 (en) |
BR (1) | BR9710199A (en) |
CA (1) | CA2259535C (en) |
DE (1) | DE69635575T2 (en) |
ES (1) | ES2253747T3 (en) |
WO (1) | WO1998001520A2 (en) |
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US6156718A (en) * | 1996-07-04 | 2000-12-05 | The Procter & Gamble Company | Process for making detergent compositions |
US6906022B1 (en) * | 1998-09-25 | 2005-06-14 | The Procter & Gamble Company | Granular detergent compositions having homogenous particles and process for producing same |
AU9585098A (en) * | 1998-09-25 | 2000-04-17 | Procter & Gamble Company, The | Granular detergent composition having improved appearance and solubility |
CA2343810A1 (en) * | 1998-09-25 | 2000-04-06 | Jacqueline Westfield | Granular detergent composition having improved appearance and solubility |
US6964945B1 (en) | 1998-09-25 | 2005-11-15 | The Procter & Gamble Company | Solid detergent compositions |
US6673766B1 (en) * | 1998-09-25 | 2004-01-06 | The Procter & Gamble Company | Solid detergent compositions containing mixtures of surfactant/builder particles |
JP2003527455A (en) * | 1998-09-25 | 2003-09-16 | ザ、プロクター、エンド、ギャンブル、カンパニー | Granular detergent composition with improved solubility properties |
JP2002528600A (en) | 1998-10-26 | 2002-09-03 | ザ、プロクター、エンド、ギャンブル、カンパニー | Method for producing a granular detergent composition having improved appearance and solubility |
EP1104804B1 (en) * | 1999-06-14 | 2005-04-20 | Kao Corporation | Method for producing single nucleus detergent particles |
CN1200999C (en) * | 1999-06-21 | 2005-05-11 | 宝洁公司 | Process for making granular detergent compsn. |
US6833346B1 (en) * | 1999-06-21 | 2004-12-21 | The Procter & Gamble Company | Process for making detergent particulates |
US6951837B1 (en) | 1999-06-21 | 2005-10-04 | The Procter & Gamble Company | Process for making a granular detergent composition |
GB0111863D0 (en) * | 2001-05-15 | 2001-07-04 | Unilever Plc | Granular composition |
DE102006029007A1 (en) * | 2006-06-24 | 2008-01-03 | Cognis Ip Management Gmbh | Solid surfactants in granular form |
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US4136051A (en) * | 1974-02-25 | 1979-01-23 | Henkel Kommanditgesellschaft Auf Aktien (Henkel Kgaa) | Pourable washing compositions containing a luminosilicates and non-ionics and method for their preparation |
JPS6189300A (en) * | 1984-10-09 | 1986-05-07 | ライオン株式会社 | Production of granular detergent composition containing nonionic surfactant |
TW240243B (en) * | 1992-03-12 | 1995-02-11 | Kao Corp | |
DE4209435A1 (en) * | 1992-03-24 | 1993-09-30 | Henkel Kgaa | Granular, non-ionic surfactants containing, phosphate-free additive for detergents and cleaners |
TR27586A (en) * | 1992-09-01 | 1995-06-13 | Procter & Gamble | Processes and compositions made with process to make high-density granular detergent. |
-
1996
- 1996-07-04 AT AT96201854T patent/ATE312901T1/en not_active IP Right Cessation
- 1996-07-04 DE DE69635575T patent/DE69635575T2/en not_active Expired - Fee Related
- 1996-07-04 EP EP96201854A patent/EP0816485B1/en not_active Expired - Lifetime
- 1996-07-04 ES ES96201854T patent/ES2253747T3/en not_active Expired - Lifetime
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1997
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- 1997-06-27 CN CNB971973946A patent/CN1195834C/en not_active Expired - Fee Related
- 1997-06-27 CA CA002259535A patent/CA2259535C/en not_active Expired - Fee Related
- 1997-06-27 WO PCT/US1997/011281 patent/WO1998001520A2/en active Application Filing
- 1997-07-03 AR ARP970102992A patent/AR008062A1/en unknown
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WO1998001520A2 (en) | 1998-01-15 |
BR9710199A (en) | 1999-11-23 |
ES2253747T3 (en) | 2006-06-01 |
DE69635575T2 (en) | 2006-09-14 |
AR008062A1 (en) | 1999-12-09 |
CN1332790A (en) | 2002-01-23 |
CN1195834C (en) | 2005-04-06 |
DE69635575D1 (en) | 2006-01-19 |
ATE312901T1 (en) | 2005-12-15 |
EP0816485A1 (en) | 1998-01-07 |
JPH11514033A (en) | 1999-11-30 |
EP0816485B1 (en) | 2005-12-14 |
CA2259535A1 (en) | 1998-01-15 |
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