CA2030306C - Detergent composition - Google Patents
Detergent compositionInfo
- Publication number
- CA2030306C CA2030306C CA002030306A CA2030306A CA2030306C CA 2030306 C CA2030306 C CA 2030306C CA 002030306 A CA002030306 A CA 002030306A CA 2030306 A CA2030306 A CA 2030306A CA 2030306 C CA2030306 C CA 2030306C
- Authority
- CA
- Canada
- Prior art keywords
- filler
- composition
- detergent active
- particulate
- anionic detergent
- 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 - Fee Related
Links
- 239000003599 detergent Substances 0.000 title claims abstract description 99
- 239000000203 mixture Substances 0.000 title claims abstract description 71
- 239000000945 filler Substances 0.000 claims abstract description 78
- 239000002245 particle Substances 0.000 claims abstract description 31
- 238000010521 absorption reaction Methods 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 21
- -1 secondary alcohol sulphates Chemical class 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 11
- 150000004996 alkyl benzenes Chemical class 0.000 claims description 8
- 239000008247 solid mixture Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 6
- 125000001273 sulfonato group Chemical group [O-]S(*)(=O)=O 0.000 claims description 5
- 239000004711 α-olefin Substances 0.000 claims description 5
- 239000011872 intimate mixture Substances 0.000 claims description 4
- 239000011369 resultant mixture Substances 0.000 claims description 4
- 230000003472 neutralizing effect Effects 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 2
- 239000011236 particulate material Substances 0.000 claims description 2
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims 3
- 150000008041 alkali metal carbonates Chemical class 0.000 claims 3
- 150000005323 carbonate salts Chemical class 0.000 claims 1
- 230000000704 physical effect Effects 0.000 abstract description 3
- 239000003921 oil Substances 0.000 description 28
- 235000019198 oils Nutrition 0.000 description 28
- 239000000843 powder Substances 0.000 description 21
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 18
- 239000000463 material Substances 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 239000008188 pellet Substances 0.000 description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 description 8
- 235000017550 sodium carbonate Nutrition 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
- 238000006386 neutralization reaction Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- 125000000129 anionic group Chemical group 0.000 description 3
- JXLHNMVSKXFWAO-UHFFFAOYSA-N azane;7-fluoro-2,1,3-benzoxadiazole-4-sulfonic acid Chemical compound N.OS(=O)(=O)C1=CC=C(F)C2=NON=C12 JXLHNMVSKXFWAO-UHFFFAOYSA-N 0.000 description 3
- JYIMWRSJCRRYNK-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4] JYIMWRSJCRRYNK-UHFFFAOYSA-N 0.000 description 3
- 229910021653 sulphate ion Inorganic materials 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 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
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 150000003138 primary alcohols Chemical class 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- OBMBUODDCOAJQP-UHFFFAOYSA-N 2-chloro-4-phenylquinoline Chemical compound C=12C=CC=CC2=NC(Cl)=CC=1C1=CC=CC=C1 OBMBUODDCOAJQP-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 241000518994 Conta Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 235000012241 calcium silicate Nutrition 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 235000019864 coconut oil Nutrition 0.000 description 1
- 239000003240 coconut oil Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 125000001924 fatty-acyl group Chemical group 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 159000000011 group IA salts Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 235000021388 linseed oil Nutrition 0.000 description 1
- 239000000944 linseed oil Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229940071207 sesquicarbonate Drugs 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000005406 washing Methods 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
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0034—Fixed on a solid conventional detergent ingredient
-
- 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
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
-
- 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
-
- 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
- C11D3/12—Water-insoluble compounds
- C11D3/14—Fillers; Abrasives ; Abrasive compositions; Suspending or absorbing agents not provided for in one single group of C11D3/12; Specific features concerning abrasives, e.g. granulometry or mixtures
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)
- Inorganic Chemistry (AREA)
- Detergent Compositions (AREA)
Abstract
A detergent composition has a high (~ 30%) content of anionic detergent yet has acceptable physical properties for use as part or all of a retail product. The anionic detergent is mixed with a particulate filler which has high oil absorbency. The filler is intimately distributed within the particles of the composition.
Description
DETERGENT COMPOSITION
FIELD AND BACKGROUND OF THE INVENTION
This invention relates to the particulate detergent compositions cont~;n;ng relatively high levels of detergent active and furthermore where the detergent comprises a high level of anionic detergent, at least 30% by weight of the composition. Such compositions may in particular be suitable for cleaning fabrics, although they may be intended for other uses. This invention also relates to the production of such compositions.
Detergent compositions containing lower levels of anionic detergent active are commonplace, and are often prepared by spray drying as is well known. At first sight it might be supposed that there would be no difficulty in making compositions with higher concentrations of anionic detergent because many anionic detergent active materials can be prepared in more or less solid form consisting of substantially pure anionic detergent, or at least containing a very high percentage of anionic detergent.
However, such materials tend to be sticky and to cake together whereas products which are suitable for retail sale are required not to be sticky and to be free flowing. A
sticky solid with a tendency to cake is of course inconvenient during manufacture as well as at the time of use.
FIELD AND BACKGROUND OF THE INVENTION
This invention relates to the particulate detergent compositions cont~;n;ng relatively high levels of detergent active and furthermore where the detergent comprises a high level of anionic detergent, at least 30% by weight of the composition. Such compositions may in particular be suitable for cleaning fabrics, although they may be intended for other uses. This invention also relates to the production of such compositions.
Detergent compositions containing lower levels of anionic detergent active are commonplace, and are often prepared by spray drying as is well known. At first sight it might be supposed that there would be no difficulty in making compositions with higher concentrations of anionic detergent because many anionic detergent active materials can be prepared in more or less solid form consisting of substantially pure anionic detergent, or at least containing a very high percentage of anionic detergent.
However, such materials tend to be sticky and to cake together whereas products which are suitable for retail sale are required not to be sticky and to be free flowing. A
sticky solid with a tendency to cake is of course inconvenient during manufacture as well as at the time of use.
2 ~o~a306 In fact it is difficult to produce a particulate solid which both contains a high proportlon of detergent active and also has satisfactory properties for use as part or the whole of a product suitable for retail sale.
SUMMARY OF THE PRIOR ART
US 4515707 (Brooks) discloses a procedure in which anionic detergent acid is neutralized and mixed with a powdered ingredient to produce a powder which is described as dry. This is used subsequently as a raw material for the production of detergent bars. The powdered ingredients which are referred to can be made with varying absorbencies and the document does not disclose materials of unusual absorbency.
US 4213874 (Williams et al) discloses the production of aluminosilicates which have an oil absorbtion of at least 75ml/lOOgram. It is disclosed that they may be used to absorb nonionic detergents in detergent products.
US 4707290, GB 1485371 and GB 1591518 disclose the use of absorbent solids to act as carriers for nonionic detergents.
Nonionic detergents are a different problem to anionic detergents in that the nonionic materials are generally liquids (which need to be made into solid form) whereby anionic detergen~ts are generally 5~ C i~ th~i- own right.
2~ It is known to apply powdered materials to the surface of a particulate solid to reduce sti~kin~cs and en~nce its abilities to flow as a powder. This however is merely a surface treatment.
SUMMARY OF THE PRIOR ART
US 4515707 (Brooks) discloses a procedure in which anionic detergent acid is neutralized and mixed with a powdered ingredient to produce a powder which is described as dry. This is used subsequently as a raw material for the production of detergent bars. The powdered ingredients which are referred to can be made with varying absorbencies and the document does not disclose materials of unusual absorbency.
US 4213874 (Williams et al) discloses the production of aluminosilicates which have an oil absorbtion of at least 75ml/lOOgram. It is disclosed that they may be used to absorb nonionic detergents in detergent products.
US 4707290, GB 1485371 and GB 1591518 disclose the use of absorbent solids to act as carriers for nonionic detergents.
Nonionic detergents are a different problem to anionic detergents in that the nonionic materials are generally liquids (which need to be made into solid form) whereby anionic detergen~ts are generally 5~ C i~ th~i- own right.
2~ It is known to apply powdered materials to the surface of a particulate solid to reduce sti~kin~cs and en~nce its abilities to flow as a powder. This however is merely a surface treatment.
3 s~ 3 0 6 THE INVENTION
We have now found that the flow properties and caking resistance of detergent powders containing a high level of anionic detergent can be improved by incorporating a particulate filler with a relatively high oil absorption value.
Accordingly, in a first aspect, the invention provides a particulate detergent composition, the particles of which contain at least 55% by weight of anionic detergent active which is any of linear and branched alkyl benzene sulphonates, alkane sulphonates, secondary alcohol sulphates, primary alcohol sulphates, alpha olefin sulphonates, alkyl ether sulphates, fatty acyl ester sulphonates, and mixtures of these, and also contain a particular filler with an oil absorption value of at least lOOml/lOOg, this filler being distributed within the particles of the composition in intimate mixture with said detergent active, and the weight ratio of the filler to the anionic detergent active lying in the range from l:lO to l:l.
In a further aspect, this invention provides a particulate detergent composition, the particles of which contain at least 30% by weight of anionic detergent active and also contain a particulate filler with an oil absorption value of at least 200ml/lOOg, this filler being distributed within the particles of the composition in intimate mixture with the detergent active, the amount of the particulate filler being such that the weight ratio of B
3 ~
the filler to anionic detergent active lies in the range from 1:10 to 1:1, more preferably 1:8 to 2:3.
This ratio range signifies that the amount of filler is not greater than the amount of anionic detergent active.
It is preferred that the filler has a mean particle size not greater than 20 micrometres.
In a still further aspect the invention provides a process of preparing a particulate detergent composition which process comprises incorporating a particulate filler into a fluid or semi-solid composition containing anionic detergent active which is any of linear and branched alkyl benzene sulphonates, alkane sulphonates, secondary alcohol sulphates, primary alcohol sulphates, alpha olefin sulphonates, alkyl ether sulphates, fatty acyl ester sulphonates, and mixtures of these so that the filler is intimately mixed with the anionic detergent active, said particulate filler having an oil absorption value in excess of lOOml/lOOgrams, and forming the resultant mixture into a particulate composition with the filler distributed within the particles of the composition, the amounts of anionic detergent active and filler being such that the composition contains at least 55 wt% of anionic detergent active ranging from 1:10 to 1:1.
A still further aspect of the invention provides a process of preparing a particulate detergent composition which process comprises incorporating a particulate filler into a fluid or semi-solid composition containing anionic B
3 ~ ~
detergent active, so that the filler is intimately mixed with the anionic detergent active, said particulate filler having an oil absorption value in excess of 200ml/lOOgrams, and forming the resultant mixture into a particulate composition with the filler distributed within the particles of the composition, the amounts of anionic detergent active and filler being such that the composition contains at least 30 wt~ of anionic detergent active and has a weight ratio of filler to anionic detergent active r~n~in~ ~ro~ 1:10 to 1~1 ",/
~B
~ Q ~ ~ 3 ~ ~
DETAILED DESC~IPTION
Test for oil absorbency As stated above, the present invention contains particulate filler with an oil absorption value which is equal to, or eX~,e~C, a minimum value.
The oil absorption value of the filler is to be determined by the following test which is in accordance with British Standard 3483 : Part B7 : 1982. The test for oil absorption is performed by placing a weighed sample of the test powder on a plate and then adding linseed oil from a burette. The oil is added a few drops at a time. After each addition the powder is mixed vigorously with the oil using a palette knife. Addition of oil is continued until a paste of smooth consistency is formed. The paste should just spread without cracking or crumbling. The oil absorption value is expressed as the volume (ml) of oil absorbed per lOO gram of powder.
Applicability of compositions ~t ~ C~r~ n ~D
~a3~3~6 - , 5 may be marketed directly as a washing product.
Alternatively it can be mixed with other particulate material to form a finished product. In particular, a particulate detergent composition according to the invention may be mixed with a second particulate composition which contains other constituents of a final detergent composition, such ~as detergency builders. There are various possibilities for such a second composition. It might contain no detergent active or very little. It might contain a substantial quantity of detergent active but nevertheless a lower proportion than in a composition according to this invention which is mixed with it.
A~ixi~g the composition in accordance with the invention would then serve to increase the overall proportion of detergent active. There could even be a commercial advantage in circumstances where ~mi xi ng a composition in accordance with this invention did not increase the overall proportion of detergent active - for instance by achieving beneficial physical properties or by e~Ancing overall production from available process plant.
Production routes Production of compositions in accordance with this invention may be ~C~l i ch~ by cuu~ on~l routss for the manufacture of part~culate detergent ro~positions with a high level of detergent active, provided there is a stage when the detergent active is in a fluid or semi-solid form.
The particulate filler is mixed with the detergent actlve at 20~3~
this stage and leads to an improvement in the properties of the particulate composition which is produced. In some inst~ es a particulate state would not be achieved without the filler.
If the overall process entails neutralization, the filler can be mixed with the acid form of the detergent active before neutralization. The filler may even be used as a base to neutralise the acid form of the detergent active, i.e. part of the material used as filler may serve to effect neutralisation. Another possibility is to neutralise the active and mix the filler with the resulting neutralised paste before this becomes solid.
A fluid or semi-solid mixture contA~ g the detergent active and the filler may be dried to solidify it, for example by means of a drum dryer. A viscous dough may be produced with a formulation such that the dough can be extruded but will then solidify into a hard solid which can be comminuted to desired particle size.
One preferred method of producing compositions of this invention is by neutralizing an acid form of an anionic detergent active with an alkali metal oxide, hydroxide or carbonate (which may be a true carbonate, bicarbonate or sesquicarbonate) to produce a viscous dough, mixing the particulate filler with this dough, allowing the dough to 2~ harden to a solid and comminuting the solid. Neutralization may be effected in the presence of little or no added water.
Alternatively there may be some ~ herate addition of water: this can lead to a solid which is already in '- 2C3~3~
equilibrium with atmospheric humidity. Generally, the amount of water added (if any) is not more than 10%, more~
preferably not more than 5%, by weight based on the total weight of acid detergent and carbonate.
Such neutralization and admixing of filler can be carried out in various types of high shear mixer. One possibility is a Z-blade mixer, another possibility is a cavity transfer mixer whose use as a chemical reactor is disclosed in our European patent application 194812, yet another possibility is a twin screw extruder. Other intensive mixers which may be used consist of vessels which contain rotating blades for mixing and high speed knives for dispersing, manufactured for example by Lodige (Trade Mark) ex Morton ~Ach~P Co Ltd, Scotland.
If production is by a route which entails neutralization of the acid form of an anionic detergent active, other detergent active may also be mixed in. For example some preneutralised detergent active or nonionic detergent active may be mixed in.
When the powder has been made it may be given a surface coating of a flow-improving aid which may itself be a particulate solid having the oil absorption property required for the filler used in this invention. Use of such materials as a surface coating is convent~o~ he 2~ eY~mplPC below demonstrate t~at it does not, by itself, achieve the results achieved by the invention.
Materials : Detergent Active 2~Q3~
As mentioned above compositions according to this invention must contain at least 30% by weight of active detergent. Preferably they contain more, e.g. at least 40%
or even at least 55~. The amount of detergent active present may range as high as 90% by weight of the composition.
Various~detergent actives may be utilised, selected from the conventional categories of anionic, nonionic, cationic and amphoteric. Preferably anionic detergent active predominates; even if detergent active from another category is present the anionic detergent active may itself provide 30%, 40% or even 55% or more of the composition.
Specific examples of anionic detergent actives useful in this invention are: linear and branched alkyl benzene sulphonates, alkane sulphonates, secondary alcohol sulphates, primary alcohol sulphates, alpha olefin sulphonates, alkyl ether sulphates, fatty acyl ester sulphonates, and mixtures of these. The invention is particularly applicable when at least part of the detergent active is alkyl benzene sulphonate, or a mixture thereof with fatty acyl ester sulphonate or primary alcohol sulphate.
Materials : Particulate Filler As stated above the filler should have an oil absorbency, measured according to the test stated, of at least lOOml/lOOg. PrefOE ably it is higher such as at least %~3Q~
150ml/lOOg, better at least 200ml/lOOg and most preferably at least 300ml/lOOg.
The filler may be water soluble but is more likely to be water insoluble.
Preferably the mean particle size of the filler is not over 20 micrometres, better not over 10 micrometres.
A small particle size is especially desirable for an insoluble filler, since it facilitates rinsing the filler away after a detergent composition has been used. Small particle size increases the speed of dissolution of a soluble filler. An alternative way to state desirable particle slze is that the particle size distribution includes substantially no particles larger than 50 micrometres. These particles however will generally be aggregates of smaller particles, typically having a size in the range from 5 to 200 nanometres and prP~om~n~tly (or even wholly) in the narrower range lO nanometres to 100 nanometres. Such smaller partlcles can be disting~1sh~ by electron microscopy.
A variety of materials are available with suitable particle size and oil absorbency. Suitable inorganic materials tend to be finely divided solids obt~i~e~ by precipitation. Materials can be produced in such form include c~l~c~ alumin~c~ tes~ calcium silicates, magnesium s~l~c~tes and calcium ~ L~. O~her materials which can be suitable, sub;ect to testing their oil absorbency, are diatomaceous earths and finely divided cellulosic fillers.
2~30~6 The amount of filler included in the composition will generally range from 3~ to 50% by weight, usually 5% to 40%.
Other materials may be included in addition to the detergent active and specified filler, for example detergency builder, alkaline salts or other filler of lesser oil absorbency. A small quantity of moisture will almost always be present.
EXAMPLES
Examples I-V and Comparative Examples A-C
A number of compositions and comparative compositions were prepared using a st~n~ard procedure as follows.
T.i ne~r alkyl benzene sulphonic acid with an average Cl 3 alkyl chain length was charged to a Z-blade mixer. Temperature was maint~i~e~ at 80~C. Sodium carbonate was added over ten minutes with continuous mixing during which time carbon dioxide was evolved. A particulate filler was then added over a period of 15 minutes and r~ xi n~ continued for 5 minutes.
The dough produced by this procedure was removed from the mixer and cut into pellets. These were allowed to cool to ambient tem~e~aL~, har~Pni n~ as they did so. The pellets were milled into a powder. This was mixed with 2%
by weight of a conventional flow aid which coated the surfaces of the powder particles.
The mean partirle s~e, bulk density and dynamic 11 ~e3~3û6 flow rate of the resulting powders were tested. Their content of sodium alkyl h~7~ne sulphonate was checked analytically and found to be approximately 60% by weight, except in Example 5 where the content was approximately 52%
by weight. The dynamic flow rate, in ml/s, was measured using a cylindrical glass tube having an internal diameter of 35mm and a len~th of 600mm. The tube was securely clamped with its longit~ axis vertical. Its lower end was terminated by means of a smooth cone of polyvinyl chloride having an internal angle of 15~ and a lower outlet orifice of diameter 22.5mm. A beam sensor was positloned 150mm above the outlet, and a second beam sensor was positioned 250mm above the first Qe~Cor.
To determine the dynamic flow rate of a powder sample, the outlet orifice was temporarily closed, for example, by covering with a piece of card, and powder was poured into the top of the cylinder until the powder level was about lOOmm above the upper s~sor. The outlet was then opened and the time t (secon~s) taken for the powder level to fall from the upper sensor to the lower sensor was measured electronically. The result is the tube volume between the se~ors, divided by the time measured.
C~k~g resistance of the particles and their hardness after e~os~e to air was tested ~y the following 2~ pr~r~ re The powder was spread in a thin layer in a dish and ~XpO~ to atmosphere at 37~C and 70% relative humidity.
After exposure for one week the powder was graded for feel.
Also a sample of the powder which had been e~ose~ was 12 ~ 3~6 compressed under a stAn~Ard load in a 2cm diameter cylindrical die to form a pellet. The hardness of the material in this pellet was tested with a cone penetrometer.
The cone had an angle of 9~ 10' and was applied under 100 gram load for 10 seconds.
The compositions of these examples and comparative examples are set QUt in Tables 1 and 2 below. In the case of comparative example A an increased quantity of sodium carbonate was used rather than a separate particulate filler. In other words a part of the sodium carbonate, having an oil absorption value of 63ml/lOOg, constituted the particulate filler. In this comparative example the sodium carbonate was added over a period of lS minutes in view of the greater quantity used.
lS The various solids were no~i nA 1 ly dry, which in practice means that they contained a small percentage of absorbed moisture.
Components Charged in the Z-blade Mixer (Kg) II III IV V A B C
5 Alkyl benzene sulphonic acid (1) 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 Sodium carbonate (2) 0.2 0.2 0.2 0.4 1.0 0.8 0.2 0.2 Water 0.020.020.02 0.02 0.02 0.020.02 0.02 *Socal U3 (3) 0.6 *Alusil ET (4) - 0.6 *Microsil GP (5) - - 0.6 0.4 0.12 *Kaolin (6) - _ 0.6 *Durcal 40 (7) - - - - - - - 0.6 (1) Sulphonated Dobane 113, ex Shell (2) Light Soda Ash, ex ICI
30 (3) Calcium Carbonate, ex Solvay (4) Aluminosilicate, ex J Crosfield and Sons (5) Silica, ex J Crosfield and Sons (6) Speswhite grade, ex English China Clays (7) Calcium Carbonate, ex Sturge.
*denotes trade mark 14 ~ Q~
Properties of Materials Produced _ II III IV V A B C_ Mean particle size (~m) 515505 465 485 510 500 515 525 Bulk density (Kg/m3) 668652 654 664 700 676 668 650 Dynamic flow rate (ml/sec) 75 80 96 96 90 75 75 70 Penetration of compacted pellet after exposure (mm) 146.8 2.4 3.5 4.2 19 20 22 Feel of the powder after exposure* S MS MC MC MC VS VS VS
Oil absorption value of the filler (ml/lOOg) 120200 330 330 330 63** 51 25 * S = Soft, MS = Moderately Soft, MC = Moderately Crisp, VS = Very Soft ** Oil absorption value of the light soda ash.
It can be seen that below an oil absorption value of lOOml/lOOg the y~o~euLies of the yO.d~l are not much affected by the oil absorption value of the filler whereas considerable i,.~ylovements are observed at higher oil absorption values.
In each case the col~en~o~l flow aid used to 2~3~30~
provide a surface coating on the particles was Alusil ET.
The inferior results with the comparative examples demonstrate that a conventional dusting or surface coating with a flow aid does not itself achieve the benefit of this invention.
Examples 6 and 7, ~Comparative Examples D and E
These Examples commence using pastes, i.e.
previously neutralised detergent active. The procedure was as follows.
Sodium primary alcohol sulphate paste or sodium alkyl h~n7~ne sulphonate paste was charged to a Z-blade mixer. Temperature was maint~ne~ at 80~C. Sodium carbonate was added over five minutes with continuous ~;~;ng. A particulate filler was then added over a period of 15 minutes and mixing continued for 5 minutes.
The dough produced by this procedure was removed from the mixer and cut into pellets. These were dried and allowed to cool to ambient temperature, hardening as they did so. Excepting pellets from Example E, which could not be milled as they were too soft, the pellets were milled into a powder. This was mixed with 2% by weight of a conventional flow aid (Alusil ET).
The physic~l properties were detP~m~ned as for 2~ Examples 1-5. The active contents were measured analytically and are shown in Table 4.
16 2~3~31~
Components charged in the Z-blade mlxer VI D VII E
5 Sodium primary alcohol sulphate paste (1) 1.0 1.0 - -Sodlum alkyl benzene sulphonate paste (~2) - - 1.0 1.0 Sodium carbonate (3) 0.25 0.4 0.45 0.6 Microsil GP (4) 0.15 - 0.15 (1) Derived from coconut oil, active content 62%.
(2) Derived from noh~e 113, ex Shell, active content 75%.
(3) Light Soda Ash, ex ICI.
(4) Silica, ex J Crosfield and Sons.
17 ~ 3~
Properties of Materials Produced VI D VII E
Moisture content after drying (%) 15.3 14.1 3.1 2.1 % Active 52 52 54 54 Mean particle size (um) 400 355 630 - (1) Bulk Density (Kg/m3) 560 585 680 Dynamic flow rate (ml/sec) 80 75 90 Penetration of comr~cted pellet after exposure (mm) 0.8 2.3 5.5 Feel of the powder after exposure (3) C MS(2) MC
Oil absorption value of the filler (ml/lOOg) 330 63 330 63 (1) Could not be satisfactorily comminuted.
(2) Formed some lumps.
(3) C = Crisp, MC = Moderately Crisp, MS = Moderately Soft.
Once again it was apparent that incorporation of filler with high oil absorption value led to powders with enhanced physical properties. Examples 7 and E are an instance where a part~ te solid was not achleved without the fil~P~,
We have now found that the flow properties and caking resistance of detergent powders containing a high level of anionic detergent can be improved by incorporating a particulate filler with a relatively high oil absorption value.
Accordingly, in a first aspect, the invention provides a particulate detergent composition, the particles of which contain at least 55% by weight of anionic detergent active which is any of linear and branched alkyl benzene sulphonates, alkane sulphonates, secondary alcohol sulphates, primary alcohol sulphates, alpha olefin sulphonates, alkyl ether sulphates, fatty acyl ester sulphonates, and mixtures of these, and also contain a particular filler with an oil absorption value of at least lOOml/lOOg, this filler being distributed within the particles of the composition in intimate mixture with said detergent active, and the weight ratio of the filler to the anionic detergent active lying in the range from l:lO to l:l.
In a further aspect, this invention provides a particulate detergent composition, the particles of which contain at least 30% by weight of anionic detergent active and also contain a particulate filler with an oil absorption value of at least 200ml/lOOg, this filler being distributed within the particles of the composition in intimate mixture with the detergent active, the amount of the particulate filler being such that the weight ratio of B
3 ~
the filler to anionic detergent active lies in the range from 1:10 to 1:1, more preferably 1:8 to 2:3.
This ratio range signifies that the amount of filler is not greater than the amount of anionic detergent active.
It is preferred that the filler has a mean particle size not greater than 20 micrometres.
In a still further aspect the invention provides a process of preparing a particulate detergent composition which process comprises incorporating a particulate filler into a fluid or semi-solid composition containing anionic detergent active which is any of linear and branched alkyl benzene sulphonates, alkane sulphonates, secondary alcohol sulphates, primary alcohol sulphates, alpha olefin sulphonates, alkyl ether sulphates, fatty acyl ester sulphonates, and mixtures of these so that the filler is intimately mixed with the anionic detergent active, said particulate filler having an oil absorption value in excess of lOOml/lOOgrams, and forming the resultant mixture into a particulate composition with the filler distributed within the particles of the composition, the amounts of anionic detergent active and filler being such that the composition contains at least 55 wt% of anionic detergent active ranging from 1:10 to 1:1.
A still further aspect of the invention provides a process of preparing a particulate detergent composition which process comprises incorporating a particulate filler into a fluid or semi-solid composition containing anionic B
3 ~ ~
detergent active, so that the filler is intimately mixed with the anionic detergent active, said particulate filler having an oil absorption value in excess of 200ml/lOOgrams, and forming the resultant mixture into a particulate composition with the filler distributed within the particles of the composition, the amounts of anionic detergent active and filler being such that the composition contains at least 30 wt~ of anionic detergent active and has a weight ratio of filler to anionic detergent active r~n~in~ ~ro~ 1:10 to 1~1 ",/
~B
~ Q ~ ~ 3 ~ ~
DETAILED DESC~IPTION
Test for oil absorbency As stated above, the present invention contains particulate filler with an oil absorption value which is equal to, or eX~,e~C, a minimum value.
The oil absorption value of the filler is to be determined by the following test which is in accordance with British Standard 3483 : Part B7 : 1982. The test for oil absorption is performed by placing a weighed sample of the test powder on a plate and then adding linseed oil from a burette. The oil is added a few drops at a time. After each addition the powder is mixed vigorously with the oil using a palette knife. Addition of oil is continued until a paste of smooth consistency is formed. The paste should just spread without cracking or crumbling. The oil absorption value is expressed as the volume (ml) of oil absorbed per lOO gram of powder.
Applicability of compositions ~t ~ C~r~ n ~D
~a3~3~6 - , 5 may be marketed directly as a washing product.
Alternatively it can be mixed with other particulate material to form a finished product. In particular, a particulate detergent composition according to the invention may be mixed with a second particulate composition which contains other constituents of a final detergent composition, such ~as detergency builders. There are various possibilities for such a second composition. It might contain no detergent active or very little. It might contain a substantial quantity of detergent active but nevertheless a lower proportion than in a composition according to this invention which is mixed with it.
A~ixi~g the composition in accordance with the invention would then serve to increase the overall proportion of detergent active. There could even be a commercial advantage in circumstances where ~mi xi ng a composition in accordance with this invention did not increase the overall proportion of detergent active - for instance by achieving beneficial physical properties or by e~Ancing overall production from available process plant.
Production routes Production of compositions in accordance with this invention may be ~C~l i ch~ by cuu~ on~l routss for the manufacture of part~culate detergent ro~positions with a high level of detergent active, provided there is a stage when the detergent active is in a fluid or semi-solid form.
The particulate filler is mixed with the detergent actlve at 20~3~
this stage and leads to an improvement in the properties of the particulate composition which is produced. In some inst~ es a particulate state would not be achieved without the filler.
If the overall process entails neutralization, the filler can be mixed with the acid form of the detergent active before neutralization. The filler may even be used as a base to neutralise the acid form of the detergent active, i.e. part of the material used as filler may serve to effect neutralisation. Another possibility is to neutralise the active and mix the filler with the resulting neutralised paste before this becomes solid.
A fluid or semi-solid mixture contA~ g the detergent active and the filler may be dried to solidify it, for example by means of a drum dryer. A viscous dough may be produced with a formulation such that the dough can be extruded but will then solidify into a hard solid which can be comminuted to desired particle size.
One preferred method of producing compositions of this invention is by neutralizing an acid form of an anionic detergent active with an alkali metal oxide, hydroxide or carbonate (which may be a true carbonate, bicarbonate or sesquicarbonate) to produce a viscous dough, mixing the particulate filler with this dough, allowing the dough to 2~ harden to a solid and comminuting the solid. Neutralization may be effected in the presence of little or no added water.
Alternatively there may be some ~ herate addition of water: this can lead to a solid which is already in '- 2C3~3~
equilibrium with atmospheric humidity. Generally, the amount of water added (if any) is not more than 10%, more~
preferably not more than 5%, by weight based on the total weight of acid detergent and carbonate.
Such neutralization and admixing of filler can be carried out in various types of high shear mixer. One possibility is a Z-blade mixer, another possibility is a cavity transfer mixer whose use as a chemical reactor is disclosed in our European patent application 194812, yet another possibility is a twin screw extruder. Other intensive mixers which may be used consist of vessels which contain rotating blades for mixing and high speed knives for dispersing, manufactured for example by Lodige (Trade Mark) ex Morton ~Ach~P Co Ltd, Scotland.
If production is by a route which entails neutralization of the acid form of an anionic detergent active, other detergent active may also be mixed in. For example some preneutralised detergent active or nonionic detergent active may be mixed in.
When the powder has been made it may be given a surface coating of a flow-improving aid which may itself be a particulate solid having the oil absorption property required for the filler used in this invention. Use of such materials as a surface coating is convent~o~ he 2~ eY~mplPC below demonstrate t~at it does not, by itself, achieve the results achieved by the invention.
Materials : Detergent Active 2~Q3~
As mentioned above compositions according to this invention must contain at least 30% by weight of active detergent. Preferably they contain more, e.g. at least 40%
or even at least 55~. The amount of detergent active present may range as high as 90% by weight of the composition.
Various~detergent actives may be utilised, selected from the conventional categories of anionic, nonionic, cationic and amphoteric. Preferably anionic detergent active predominates; even if detergent active from another category is present the anionic detergent active may itself provide 30%, 40% or even 55% or more of the composition.
Specific examples of anionic detergent actives useful in this invention are: linear and branched alkyl benzene sulphonates, alkane sulphonates, secondary alcohol sulphates, primary alcohol sulphates, alpha olefin sulphonates, alkyl ether sulphates, fatty acyl ester sulphonates, and mixtures of these. The invention is particularly applicable when at least part of the detergent active is alkyl benzene sulphonate, or a mixture thereof with fatty acyl ester sulphonate or primary alcohol sulphate.
Materials : Particulate Filler As stated above the filler should have an oil absorbency, measured according to the test stated, of at least lOOml/lOOg. PrefOE ably it is higher such as at least %~3Q~
150ml/lOOg, better at least 200ml/lOOg and most preferably at least 300ml/lOOg.
The filler may be water soluble but is more likely to be water insoluble.
Preferably the mean particle size of the filler is not over 20 micrometres, better not over 10 micrometres.
A small particle size is especially desirable for an insoluble filler, since it facilitates rinsing the filler away after a detergent composition has been used. Small particle size increases the speed of dissolution of a soluble filler. An alternative way to state desirable particle slze is that the particle size distribution includes substantially no particles larger than 50 micrometres. These particles however will generally be aggregates of smaller particles, typically having a size in the range from 5 to 200 nanometres and prP~om~n~tly (or even wholly) in the narrower range lO nanometres to 100 nanometres. Such smaller partlcles can be disting~1sh~ by electron microscopy.
A variety of materials are available with suitable particle size and oil absorbency. Suitable inorganic materials tend to be finely divided solids obt~i~e~ by precipitation. Materials can be produced in such form include c~l~c~ alumin~c~ tes~ calcium silicates, magnesium s~l~c~tes and calcium ~ L~. O~her materials which can be suitable, sub;ect to testing their oil absorbency, are diatomaceous earths and finely divided cellulosic fillers.
2~30~6 The amount of filler included in the composition will generally range from 3~ to 50% by weight, usually 5% to 40%.
Other materials may be included in addition to the detergent active and specified filler, for example detergency builder, alkaline salts or other filler of lesser oil absorbency. A small quantity of moisture will almost always be present.
EXAMPLES
Examples I-V and Comparative Examples A-C
A number of compositions and comparative compositions were prepared using a st~n~ard procedure as follows.
T.i ne~r alkyl benzene sulphonic acid with an average Cl 3 alkyl chain length was charged to a Z-blade mixer. Temperature was maint~i~e~ at 80~C. Sodium carbonate was added over ten minutes with continuous mixing during which time carbon dioxide was evolved. A particulate filler was then added over a period of 15 minutes and r~ xi n~ continued for 5 minutes.
The dough produced by this procedure was removed from the mixer and cut into pellets. These were allowed to cool to ambient tem~e~aL~, har~Pni n~ as they did so. The pellets were milled into a powder. This was mixed with 2%
by weight of a conventional flow aid which coated the surfaces of the powder particles.
The mean partirle s~e, bulk density and dynamic 11 ~e3~3û6 flow rate of the resulting powders were tested. Their content of sodium alkyl h~7~ne sulphonate was checked analytically and found to be approximately 60% by weight, except in Example 5 where the content was approximately 52%
by weight. The dynamic flow rate, in ml/s, was measured using a cylindrical glass tube having an internal diameter of 35mm and a len~th of 600mm. The tube was securely clamped with its longit~ axis vertical. Its lower end was terminated by means of a smooth cone of polyvinyl chloride having an internal angle of 15~ and a lower outlet orifice of diameter 22.5mm. A beam sensor was positloned 150mm above the outlet, and a second beam sensor was positioned 250mm above the first Qe~Cor.
To determine the dynamic flow rate of a powder sample, the outlet orifice was temporarily closed, for example, by covering with a piece of card, and powder was poured into the top of the cylinder until the powder level was about lOOmm above the upper s~sor. The outlet was then opened and the time t (secon~s) taken for the powder level to fall from the upper sensor to the lower sensor was measured electronically. The result is the tube volume between the se~ors, divided by the time measured.
C~k~g resistance of the particles and their hardness after e~os~e to air was tested ~y the following 2~ pr~r~ re The powder was spread in a thin layer in a dish and ~XpO~ to atmosphere at 37~C and 70% relative humidity.
After exposure for one week the powder was graded for feel.
Also a sample of the powder which had been e~ose~ was 12 ~ 3~6 compressed under a stAn~Ard load in a 2cm diameter cylindrical die to form a pellet. The hardness of the material in this pellet was tested with a cone penetrometer.
The cone had an angle of 9~ 10' and was applied under 100 gram load for 10 seconds.
The compositions of these examples and comparative examples are set QUt in Tables 1 and 2 below. In the case of comparative example A an increased quantity of sodium carbonate was used rather than a separate particulate filler. In other words a part of the sodium carbonate, having an oil absorption value of 63ml/lOOg, constituted the particulate filler. In this comparative example the sodium carbonate was added over a period of lS minutes in view of the greater quantity used.
lS The various solids were no~i nA 1 ly dry, which in practice means that they contained a small percentage of absorbed moisture.
Components Charged in the Z-blade Mixer (Kg) II III IV V A B C
5 Alkyl benzene sulphonic acid (1) 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 Sodium carbonate (2) 0.2 0.2 0.2 0.4 1.0 0.8 0.2 0.2 Water 0.020.020.02 0.02 0.02 0.020.02 0.02 *Socal U3 (3) 0.6 *Alusil ET (4) - 0.6 *Microsil GP (5) - - 0.6 0.4 0.12 *Kaolin (6) - _ 0.6 *Durcal 40 (7) - - - - - - - 0.6 (1) Sulphonated Dobane 113, ex Shell (2) Light Soda Ash, ex ICI
30 (3) Calcium Carbonate, ex Solvay (4) Aluminosilicate, ex J Crosfield and Sons (5) Silica, ex J Crosfield and Sons (6) Speswhite grade, ex English China Clays (7) Calcium Carbonate, ex Sturge.
*denotes trade mark 14 ~ Q~
Properties of Materials Produced _ II III IV V A B C_ Mean particle size (~m) 515505 465 485 510 500 515 525 Bulk density (Kg/m3) 668652 654 664 700 676 668 650 Dynamic flow rate (ml/sec) 75 80 96 96 90 75 75 70 Penetration of compacted pellet after exposure (mm) 146.8 2.4 3.5 4.2 19 20 22 Feel of the powder after exposure* S MS MC MC MC VS VS VS
Oil absorption value of the filler (ml/lOOg) 120200 330 330 330 63** 51 25 * S = Soft, MS = Moderately Soft, MC = Moderately Crisp, VS = Very Soft ** Oil absorption value of the light soda ash.
It can be seen that below an oil absorption value of lOOml/lOOg the y~o~euLies of the yO.d~l are not much affected by the oil absorption value of the filler whereas considerable i,.~ylovements are observed at higher oil absorption values.
In each case the col~en~o~l flow aid used to 2~3~30~
provide a surface coating on the particles was Alusil ET.
The inferior results with the comparative examples demonstrate that a conventional dusting or surface coating with a flow aid does not itself achieve the benefit of this invention.
Examples 6 and 7, ~Comparative Examples D and E
These Examples commence using pastes, i.e.
previously neutralised detergent active. The procedure was as follows.
Sodium primary alcohol sulphate paste or sodium alkyl h~n7~ne sulphonate paste was charged to a Z-blade mixer. Temperature was maint~ne~ at 80~C. Sodium carbonate was added over five minutes with continuous ~;~;ng. A particulate filler was then added over a period of 15 minutes and mixing continued for 5 minutes.
The dough produced by this procedure was removed from the mixer and cut into pellets. These were dried and allowed to cool to ambient temperature, hardening as they did so. Excepting pellets from Example E, which could not be milled as they were too soft, the pellets were milled into a powder. This was mixed with 2% by weight of a conventional flow aid (Alusil ET).
The physic~l properties were detP~m~ned as for 2~ Examples 1-5. The active contents were measured analytically and are shown in Table 4.
16 2~3~31~
Components charged in the Z-blade mlxer VI D VII E
5 Sodium primary alcohol sulphate paste (1) 1.0 1.0 - -Sodlum alkyl benzene sulphonate paste (~2) - - 1.0 1.0 Sodium carbonate (3) 0.25 0.4 0.45 0.6 Microsil GP (4) 0.15 - 0.15 (1) Derived from coconut oil, active content 62%.
(2) Derived from noh~e 113, ex Shell, active content 75%.
(3) Light Soda Ash, ex ICI.
(4) Silica, ex J Crosfield and Sons.
17 ~ 3~
Properties of Materials Produced VI D VII E
Moisture content after drying (%) 15.3 14.1 3.1 2.1 % Active 52 52 54 54 Mean particle size (um) 400 355 630 - (1) Bulk Density (Kg/m3) 560 585 680 Dynamic flow rate (ml/sec) 80 75 90 Penetration of comr~cted pellet after exposure (mm) 0.8 2.3 5.5 Feel of the powder after exposure (3) C MS(2) MC
Oil absorption value of the filler (ml/lOOg) 330 63 330 63 (1) Could not be satisfactorily comminuted.
(2) Formed some lumps.
(3) C = Crisp, MC = Moderately Crisp, MS = Moderately Soft.
Once again it was apparent that incorporation of filler with high oil absorption value led to powders with enhanced physical properties. Examples 7 and E are an instance where a part~ te solid was not achleved without the fil~P~,
Claims (11)
1. A particulate detergent composition, the particles of which contain at least 55% by weight of anionic detergent active which is any of linear and branched alkyl benzene sulphonates, alkane sulphonates, secondary alcohol sulphates, primary alcohol sulphates, alpha olefin sulphonates, alkyl ether sulphates, fatty acyl ester sulphonates, and mixtures of these, and also contain a particulate filler with an oil absorption value of at least 100ml/100g, this filler being distributed within the particles of the composition in intimate mixture with said detergent active, and the weight ratio of the filler to the anionic detergent active lying in the range from 1:10 to 1:1.
2. A particulate detergent composition, the particles of which contain at least 30% by weight of anionic detergent active and also contain a particulate filler with an oil absorption value of at least 200ml/100g, this filler being distributed within the particles of the composition in intimate mixture with said detergent active, and the weight ratio of the filler to the anionic detergent active lying in the range from 1:10 to 1:1.
3. A composition according to claim 1 or claim 2 wherein the filler has a mean particle size not greater than 20 micrometres.
4. A composition according to claim 1 or claim 2 wherein the filler is water-insoluble.
5. A composition according to claim 1 or claim 2 wherein the filler has a particulate size distribution such that substantially no filler particles have a size greater than 50 micrometres.
6. A mixture comprising a composition according to claim 1 or claim 2 together with other solid particulate material, in an amount such that the mixture contains 3 to 50% by weight of said filler.
7. A process of preparing a particulate detergent composition which process comprises incorporating a particulate filler into a fluid or semi-solid composition containing anionic detergent active which is any of linear and branched alkyl benzene sulphonates, alkane sulphonates, secondary alcohol sulphates, primary alcohol sulphates, alpha olefin sulphonates, alkyl ether sulphates, fatty acyl ester sulphonates, and mixtures of these so that the filler is intimately mixed with the anionic detergent active, said particulate filler having an oil absorption value in excess of 100ml/100grams, and forming the resultant mixture into a particulate composition with the filler distributed within the particles of the composition, the amounts of anionic detergent active and filler being such that the composition contains at least 55 wt% of anionic detergent active ranging from 1:10 to 1:1.
8. A process according to claim 7 comprising neutralizing the acid form of anionic detergent active with an alkali metal carbonate salt to form a semi-solid composition containing the neutralized detergent active, said filler then being added to the said composition, the process thereafter comprising allowing the resulting mixture to harden, and comminuting it.
9. A process of preparing a particulate detergent composition which process comprises incorporating a particulate filler into a fluid or semi-solid composition containing anionic detergent active, so that the filler is intimately mixed with the anionic detergent active, said particulate filler having an oil absorption value in excess of 200ml/100grams, and forming the resultant mixture into a particulate composition with the filler distributed within the particles of the composition, the amounts of anionic detergent active and filler being such that the composition contains at least 30 wt% of anionic detergent active and has a weight ratio of filler to anionic detergent active ranging from 1:10 to 1:1.
10. A process according to claim 9 comprising neutralizing the acid form of anionic detergent active with an alkali metal carbonate salt to form a semi-solid composition containing the neutralized detergent active, said filler then being added to the said composition, the process thereafter comprising allowing the resulting mixture to harden, and comminuting it.
11. A process according to claim 8 or claim 10 wherein the amount of water (if any) added to the acid form of the anionic detergent active and the alkali metal carbonate salt is not more than 10% by weight based on the total of the acid and the carbonate salt.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB8926644.9 | 1989-11-24 | ||
| GB898926644A GB8926644D0 (en) | 1989-11-24 | 1989-11-24 | Detergent composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CA2030306A1 CA2030306A1 (en) | 1991-05-25 |
| CA2030306C true CA2030306C (en) | 1998-12-22 |
Family
ID=10666891
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002030306A Expired - Fee Related CA2030306C (en) | 1989-11-24 | 1990-11-20 | Detergent composition |
Country Status (10)
| Country | Link |
|---|---|
| EP (1) | EP0430603B1 (en) |
| JP (1) | JPH03177499A (en) |
| AU (1) | AU629429B2 (en) |
| BR (1) | BR9005872A (en) |
| CA (1) | CA2030306C (en) |
| DE (1) | DE69016374T2 (en) |
| ES (1) | ES2067699T3 (en) |
| GB (1) | GB8926644D0 (en) |
| NO (1) | NO176405C (en) |
| ZA (1) | ZA909423B (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2721616A1 (en) | 1994-06-22 | 1995-12-29 | Hoechst France | Compositions of anionic surfactants in powder, pearls or granules, process for their preparation and their use in cleaning and maintenance products |
| DE4440621A1 (en) * | 1994-11-14 | 1996-05-15 | Henkel Kgaa | Scouring powder with improved flow properties and process for its production |
| GB9825558D0 (en) * | 1998-11-20 | 1999-01-13 | Unilever Plc | Granular detergent components and particulate detergent compositions containing them |
| DE19961687A1 (en) * | 1999-12-21 | 2001-07-05 | Henkel Kgaa | Combination of active ingredients for incorporation in detergents and cleaners |
| WO2014198034A1 (en) * | 2013-06-13 | 2014-12-18 | The Procter & Gamble Company | Granular laundry detergent |
| US9828569B2 (en) | 2013-06-13 | 2017-11-28 | The Procter & Gamble Company | Granular laundry detergent |
| ES2718092T3 (en) | 2013-07-18 | 2019-06-27 | Galaxy Surfactants Ltd | Alkyl ether sulfates highly active solid that flow freely |
| EP3271444A1 (en) * | 2015-03-19 | 2018-01-24 | The Procter and Gamble Company | Structured detergent particles and granular detergent compositions containing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL200200A (en) * | 1954-09-06 | |||
| ES441319A1 (en) * | 1974-09-27 | 1977-07-01 | Procter & Gamble | Funmukansoshita tansankarushiumuganjukaryu |
| US4049586A (en) * | 1974-09-27 | 1977-09-20 | The Procter & Gamble Company | Builder system and detergent product |
| GB1583081A (en) * | 1977-05-18 | 1981-01-21 | Unilever Ltd | Production of detergent compositions |
| ES8607378A1 (en) * | 1984-08-06 | 1986-05-16 | Kao Corp | Powder detergent of high density |
| US4919847A (en) * | 1988-06-03 | 1990-04-24 | Colgate Palmolive Co. | Process for manufacturing particulate detergent composition directly from in situ produced anionic detergent salt |
-
1989
- 1989-11-24 GB GB898926644A patent/GB8926644D0/en active Pending
-
1990
- 1990-11-20 CA CA002030306A patent/CA2030306C/en not_active Expired - Fee Related
- 1990-11-20 BR BR909005872A patent/BR9005872A/en not_active IP Right Cessation
- 1990-11-22 JP JP2320525A patent/JPH03177499A/en active Pending
- 1990-11-22 AU AU66899/90A patent/AU629429B2/en not_active Ceased
- 1990-11-23 ES ES90312779T patent/ES2067699T3/en not_active Expired - Lifetime
- 1990-11-23 ZA ZA909423A patent/ZA909423B/en unknown
- 1990-11-23 DE DE69016374T patent/DE69016374T2/en not_active Revoked
- 1990-11-23 NO NO905080A patent/NO176405C/en not_active IP Right Cessation
- 1990-11-23 EP EP90312779A patent/EP0430603B1/en not_active Revoked
Also Published As
| Publication number | Publication date |
|---|---|
| NO905080L (en) | 1991-05-27 |
| CA2030306A1 (en) | 1991-05-25 |
| JPH03177499A (en) | 1991-08-01 |
| ZA909423B (en) | 1992-07-29 |
| AU629429B2 (en) | 1992-10-01 |
| EP0430603A2 (en) | 1991-06-05 |
| EP0430603B1 (en) | 1995-01-25 |
| BR9005872A (en) | 1991-09-24 |
| NO905080D0 (en) | 1990-11-23 |
| ES2067699T3 (en) | 1995-04-01 |
| AU6689990A (en) | 1991-05-30 |
| DE69016374T2 (en) | 1995-05-24 |
| NO176405C (en) | 1995-03-29 |
| NO176405B (en) | 1994-12-19 |
| EP0430603A3 (en) | 1991-11-27 |
| GB8926644D0 (en) | 1990-01-17 |
| DE69016374D1 (en) | 1995-03-09 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EEER | Examination request | ||
| MKLA | Lapsed |