GB2242909A - A process for preparing granules for detergent compositions - Google Patents

A process for preparing granules for detergent compositions Download PDF

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Publication number
GB2242909A
GB2242909A GB9106793A GB9106793A GB2242909A GB 2242909 A GB2242909 A GB 2242909A GB 9106793 A GB9106793 A GB 9106793A GB 9106793 A GB9106793 A GB 9106793A GB 2242909 A GB2242909 A GB 2242909A
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GB
United Kingdom
Prior art keywords
granules
zeolite
process according
smectite clay
finely divided
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.)
Granted
Application number
GB9106793A
Other versions
GB2242909B (en
GB9106793D0 (en
Inventor
Howard Goodman
Gary Arthur Lymath
David John Stockley
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Imerys Minerals Ltd
Original Assignee
ECC International Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by ECC International Ltd filed Critical ECC International Ltd
Publication of GB9106793D0 publication Critical patent/GB9106793D0/en
Publication of GB2242909A publication Critical patent/GB2242909A/en
Application granted granted Critical
Publication of GB2242909B publication Critical patent/GB2242909B/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions
    • C11D11/0082Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions 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
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/12Water-insoluble compounds
    • C11D3/124Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246Silicates, e.g. diatomaceous earth
    • C11D3/1253Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
    • C11D3/1266Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite in liquid compositions
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/12Water-insoluble compounds
    • C11D3/124Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246Silicates, e.g. diatomaceous earth
    • C11D3/128Aluminium silicates, e.g. zeolites

Description

0 1 A PROCESS FOR PREPARING GRANULES FOR DETERGENT COMPOSITIONS This
invention relates to a process for preparing granules for incorporation into detergent compositions and, in particular, to a process for preparing granules comprising a zeolite; and to detergent composition containing the granules produced by the process.
It is generally desirable that the components of a detergent composition should be in granule form because the bulk density of a granular composition is higher than that of a finely divided powder with the result that a given weight of the composition can be packed into a smaller container when the composition is granular than when it is in powder form.
The granules should be free flowing and should also be resistant to crushing and abrasion so that they can withstand handling and transportation in containers. They should also be relatively white in colour and will typically have sizes in the range of from 0.75mm to 2.Omm.
Zeolite, which is a cation exchanging aluminosilicate, is included in detergent compositions to perform the function of a builder or scavenger of metal cations, especially calcium and magnesium ions, from the washing water, which ions, if allowed to remain in solution, would impair the effectiveness of the surfactant present in the detergent composition. Until recent years the function of the builder in detergent compositions has been fulfilled by water-' soluble condensed phosphate salts, for example sodium hexametaphosphates, but the discharge of large quantities of phosphates into rivers is damaging to the environment, and there is therefore a growing trend towards replacing phosphate builders with zeolites. A zeolite with a particularly advantageous cation exchange capacity is known as zeolite A or zeolite 4A, 1 1 and it is this zeolite which is commonly found in detergent compositions. Zeolite A is generally available in commerce in the form of a fine powder having particles of size of the order of a few microns, 5 but it has hitherto been found difficult to form the zeolite into granules of suitable size which are sufficiently coherent to withstand handling and transportation in packages without the use of additional binding materials which add to the expense and are undesirable in the complete detergent compositions. An attempt to overcome this problem is disclosed in EP-A-0279040 in which the detergent builder is prepared by spray-drying a feed suspension containing the zeolite and bentonite.
A smectite clay, for example bentonite, is often included in a detergent composition. The clay may be included on account of its fabric softening properties, or as a stabilising agent for the detergent composition, but the use of the clay brings with it the disadvantage that the clay is somewhat dark in colour and therefore imparts an undesirable dark colouration to the composition containing it. According to one aspect of the invention there is provided a process for preparing a granule for incorporation in a detergent composition, which process comprises the steps of (a) tumbling together in a rotating pan a finely divided, particulate smectite clay and a finely divided, particulate zeolite in a weight ratio of 30 from 1:9 to 9:1 whilst sufficient water is added slowly to the resultant mixture to bind the particles together to form granules of a mixture of said smectite clay and said zeolite; and (b) drying the resultant granules to reduce the water content to not more than 20% of the total weight of the granules.
V1 1 The process of the invention preferably includes the further step of:
(c). sieving the dried granules to yield a product comprising granules having sizes in the range from 0.75mm to 2.Omm.
Granules prepared in accordance with the invention are solid and will comprise the smectite clay and zeolite in a weight ratio of from 1:9 to 9:1.
The present invention also provides a detergent composition which includes granules prepared in accordance with the process of the present invention. The detergent composition will contain a surfactant and optionally other ingredients in amounts known per se.
The smectite clay may be montmorillonite, saponite, hectorite, nontronite or beidellite, but is most conveniently a bentonite clay which is a naturally occurring clay of volcanic origins consisting predominantly of montmorillonite.
The weight ratio of zeolite to smectite clay charged to the pan may preferably be in the range of from 2:8 to 8:2, more preferably 3:7 to 7:3, especially 7:3.
The smectite clay in its initial, finely divided, particulate form preferably has a particle size distribution such that substantially all of it passes through a No. 60 mesh British Standard sieve (nominal aperture 0.250mm).
The zeolite is most advantageously a synthetic zeolite such as zeolite A which has a chemical composition corresponding to the approximate formula:- 1.0+0.2 Na20. A1203. 1-9+O'l S'021 0-5.1H20 and an apparent pore width of approximately 4 Angstrom units. Preferably, the initial, finely divided, particulate zeolite has a particle size distribution such that it consists predominantly of particles having sizes in the range from 1 to 10 microns.
The granules of the present invention may also incorporate minor proportions of other ingredients, and up to 20 of the total weight of the granules may be water (as residual water derived either from the water binder added or moisture present in either of the clay or zeolite components). No additional liquid binder material is essential to form the granules; i.e. the water used in step (a) is preferably the sole liquid binder employed. The size of the final granules, after sieving is preferably from 0.75mm to 2.Omm, most preferably from 0.85mm to 1.7mm. Also, the granules preferably should not contain more than about 7% by weight of particles smaller than 0.15mm.
In the process of the invention, the smectite clay and the zeolite are preferably tumbled together in a pan granulator. The Eirich pan granulator is an example of a particularly suitable device. The quantities of zeolite and smectite clay added to the pan are those necessary to give the desired proportions of each component in the resultant granules and this will normally mean that from 10 to 90% by weight of smectite clay and from 90 to 10% by weight of zeolite are added, based on the total weight of smectite clay and zeolite. The water is preferably added in the form of a fine spray and in an amount such that it constitutes preferably at least 10% and preferably no more than 40% of the total weight of the granules formed in step (a) of the process. Thus, for every 100 parts by weight of smectite clay/zeolite mixture charged to the pan, from about 11 to about 67 parts by weight of water may be employed.
The granules may conveniently be thermally dried in step (b) in, for example, a f luidised bed dryer.
The process of the present invention provides granules which are sufficiently coherent to withstand handling and transportation in containers without the 1 use of an additional binding material. It is believed that the smectite clay itself acts as a binder which makes it possible to form,coherent granules containing a zeolite. The granules of the invention also have the advantages of being relatively light in colour compared with the smectite clay on its own.
A typical, conventional detergent composition contains the following ingredients normally in amounts in the ranges given below:
Ingredient by weight Anionic surfactant 1 - 30 Nonionic surfactant 1 - 17 Suds controlling agent Zeolite A Sodium carbonate Bleaching agent Smectite clay Cellulose ether Enzymes Optical brightening agent Sodium silicate Formulation aid Water 0 1 10 0 1 0 - 0.5 0 - 2.5 0.05 - 0.25 0 -25 0 - 1 to 100 With the present invention, at least part of the Zeolite A and at least part of the smectite clay in the foregoing composition can be replaced by granules in accordance with the present invention.
The anionic surfactant may be, for example, an alkyl benzene sulphonate or a fatty alcohol ether sulphate.
The nonionic surfactant may be, for example, an alkyl polyethyleneglycol ether or a nonylphenol polyethyleneglycol ether.
The suds controlling agent may be, for example, a soap, a silicone oil or a paraffin.
The bleaching agent may be, for example, sodium - 0.6 - 45 perborate or sodium percarbonate.
The invention is illustrated by the following Example.
EXAMPLE
A bentonite clay having a particle size distribution such that 99% by weight passed a No. 60 mesh British Standard sieve (nominal aperture 0.250mm) and 85% by weight passed a No. 200 mesh British Standard sieve (nominal aperture 0.076mm) and a zeolite A powder having a particle size distribution such that 70% by weight consisted of particles in the range from 2 to 6 microns were loaded into the pan of an Eirich granulator in the proportions 70% by weight of zeolite and 30 by weight of bentonite. The pan was set in motion at a speed of 46 rpm and the agitator at a speed of 1429m.min-1 and the clay and zeolite were mixed in a substantially dry state for 15 seconds. During the next 10 seconds, with the pan and agitator rotating at the same speeds, sufficient water was sprayed on to the mixture of clay and zeolite to give a final water content of the granules of 33% by weight. Finally the moist granules were tumbled in the pan of the granulator for a further 75 seconds at the same speed settings for the pan and for the agitator.
The moist granules were then dried in a fluidised bed dryer at a temperature of 800C for a time sufficient to reduce the water content of the granules to 14% by weight. The granules were then screened on a sieve having a nominal aperture size of 1.2mm and the granules passing through the sieve were retained as the product. The starting materials and the product granules were tested for bulk density and for reflectance to violet light of wavelength 457= and the results obtained are set forth in the following Table:
:i v 1 J.
1 w granule TABLE
Bulk density (cl. cm-'j % reflectance to light of 457nm wavelenth powder Bentonite 0.70 76.0 53.0 Zeolite A 0.50 94.5 - Bentonite/zeolite A granule 0.73 - 77.1 The granules were found to be sufficiently coherent to be able to withstand bulk handling and transportation in containers, and the reflectance to violet light of 457nm wavelength of 77.1 was sufficiently high to give the granules an acceptably light colour 'such that they would not impair the white appearance of a detergent composition in which they were incorporated.
i

Claims (11)

1. A process for preparing granules for incorporation into a detergent composition, which process comprises the steps of (a) tumbling together in a rotating pan a finely divided particulate smectite clay and a finely divided particulate zeolite in a weight ratio of from 1:9 to 9:1 whilst sufficient water is added slowly to the resultant mixture to bind the particles together to form granules of a mixture of said smectite clay and said zeolite; and (b) drying the resultant granules to reduce the water content to not more than 20 of the total weight of the granules.
2. A process according to claim 1 wherein the smectite clay is a bentonite clay.
3. A process according to claim 1 or 2 wherein the smectite clay in its initial, finely divided, particulate form has a particle size distribution such that substantially all of it passes through a No. 60 mesh British Standard sieve (nominal aperture 0.250mm).
4. A process according to any one of claims 1 to 3, wherein the zeolite is zeolite A.
5. A process according to claim 3, wherein the zeolite A has a chemical composition corresponding to the approximate formula:1.0+0.2 Na20. A1203. 1-9+0-1 S'021 0-5.1H20 and an apparent pore width of approximately 4 Angstrom units. 30
6. A process according to any preceding claim, wherein the initial, finely divided, particulate zeolite has a particle size distribution such that it consists predominantly of particles having sizes in the range from 1 to 10 microns. 35
7. A process according to any one of the preceding claims, wherein the water added in step (a) t i 1 1 e is the sole liquid binder.
8. A process according'to any one of the preceding claims, comprising the following further step: (c) sieving'the dried granules to yield a product comprising granules having sizes in the range from 0.75mm to 2.Omm.
9. A detergent composition including granules prepared by the following process: 10 (a) tumbling together in a rotating pan a finely divided particulate smectite clay and a finely divided particulate zeolite in a weight ratio of from 1:9 to 9:1 whilst sufficient water is added slowly to the resultant mixture to bind the 15 particles together to form granules of a mixture of said smectite clay and said zeolite; and (b) drying the resultant granules to reduce the water content to not more than 20% of the total weight of the granules. 20
10. A process for preparing granules for incorporation into a detergent composition substantially as hereinbefore described, with reference to the accompanying Example.
11. A detergent composition substantially as hereinbefore described, with reference to the -accompanying Example.
Published 3991 at The Patent Office. Concept House. Cardiff Road. Newport. Gwent NP9 1 RH. Further copies may be obtained from Sales Branch. Unit 6. Nine Mile Point. CwTnfelinfach. Cross Keys. Newport. NP1 7HZ. Printed by Multiplex techniques lid, St Mary Cray. Kent.
GB9106793A 1990-04-12 1991-04-02 A process for preparing granules for detergent compositions Expired - Fee Related GB2242909B (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB909008462A GB9008462D0 (en) 1990-04-12 1990-04-12 Granules for detergent compositions

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GB9106793D0 GB9106793D0 (en) 1991-05-22
GB2242909A true GB2242909A (en) 1991-10-16
GB2242909B GB2242909B (en) 1993-07-07

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GB909008462A Pending GB9008462D0 (en) 1990-04-12 1990-04-12 Granules for detergent compositions
GB9106793A Expired - Fee Related GB2242909B (en) 1990-04-12 1991-04-02 A process for preparing granules for detergent compositions

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GB909008462A Pending GB9008462D0 (en) 1990-04-12 1990-04-12 Granules for detergent compositions

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EP (1) EP0452016A3 (en)
JP (1) JPH04225098A (en)
AU (1) AU642230B2 (en)
CA (1) CA2040050A1 (en)
GB (2) GB9008462D0 (en)
NZ (1) NZ237774A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2297977A (en) * 1995-02-07 1996-08-21 Procter & Gamble Detergent composition containing Zeolite MAP

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4210253A1 (en) * 1992-03-28 1993-09-30 Hoechst Ag Cogranulates consisting of aluminosilicates and sodium silicates, a process for their preparation and their use
DE4306665A1 (en) * 1993-03-03 1994-09-08 Sued Chemie Ag Detergent additive for fabric softening detergents
EP0627484A1 (en) * 1993-06-02 1994-12-07 The Procter & Gamble Company Coating clay agglomerates with finely divided particulate material
JP4120766B2 (en) 1999-11-29 2008-07-16 株式会社アイキュ−センタ− Cleaning composition and method for producing the same

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0279040A1 (en) * 1987-01-30 1988-08-24 Degussa Aktiengesellschaft Builder for washing agents

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3060548D1 (en) * 1979-06-18 1982-08-05 Pq Corp Agglomerated zeolite ion exchanger
AU549000B2 (en) * 1981-02-26 1986-01-09 Colgate-Palmolive Pty. Ltd. Base beads for detergent compositions
AU549122B2 (en) * 1981-02-26 1986-01-16 Colgate-Palmolive Pty. Ltd. Spray dried base beads and detergent compositions
DE3620009A1 (en) * 1986-06-13 1987-12-17 Henkel Kgaa CLEANING AGENTS CONTAINING KOERNIG AGGLOMERED SODIUM METASILICATE, METHOD FOR THE PRODUCTION AND USE THEREOF

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0279040A1 (en) * 1987-01-30 1988-08-24 Degussa Aktiengesellschaft Builder for washing agents

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2297977A (en) * 1995-02-07 1996-08-21 Procter & Gamble Detergent composition containing Zeolite MAP

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AU7432591A (en) 1991-10-17
GB2242909B (en) 1993-07-07
CA2040050A1 (en) 1991-10-13
GB9008462D0 (en) 1990-06-13
JPH04225098A (en) 1992-08-14
NZ237774A (en) 1993-07-27
EP0452016A3 (en) 1992-03-11
EP0452016A2 (en) 1991-10-16
GB9106793D0 (en) 1991-05-22
AU642230B2 (en) 1993-10-14

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PCNP Patent ceased through non-payment of renewal fee

Effective date: 19950402