US3759834A - Detergent composition - Google Patents

Abstract

A TRANSLUCENT NON-BRITTLE DETERGENT FLAKE HAVING IMPROVED PROPERTIES CONTAINS FROM 70 TO 95 PERCENT BY WEIGHT OF AN ALKALI-METAL C8-C22, PREFERABLY C14 TO C16, ALPHA-OLEFIN SULPHONATE AND FROM 5 TO 11 PERCENT BY WEIGHT OF WATER. THE FLAKE CAN OPTIONALLY CONTAIN MINOR AMOUNTS OF OTHER NON-SOAP DETERGENT ACTIVE AGENTS, SOAPS, AND DETERGENCY BUILDERS, PARTICULARLY TRISODIUM NITRILOTRIACETATE.

Description

United States Patent U.S. Cl. 252-110 6 Claims ABSTRACT OF THE DISCLOSURE A translucent, non-brittle detergent flake having improved properties contains from 70 to 95 percent by weight of an alkali-metal C -C preferably C to C alpha-olefin sulphonate and from 5 to 11 percent by weight of water. The flake can optionally contain minor amounts of other non-soap detergent active agents, soaps, and detergency builders, particularly trisodium nitrilotriacetate.

This patent application is a continuation-in-part application of copending application Ser. No. 74,241 filed Sept. 21, 1970, now abandoned, which is itself is a continuation-in-part application of copending application Ser. No. 705,021 filed Feb. 13, 1968, now abandoned.

FIELD OF THE INVENTION This invention relates to detergent flakes containing a major amount of non-soap detergent active agents.

BACKGROUND OF THE INVENTION Soap flakes are very well known and are reasonably easy to manufacture, but satisfactory detergent flakes are diflicult to make. Even when a detergent flake can be milled sufliciently thinly, the flakes so obtained tend to be opaque and brittle and have unsatisfactory lathering properties. These problems are particularly acute if the detergent flake contains a detergency builder such as sodium tripolyphosphate.

Soap flakes and detergent flakes can vary in size, but to be satisfactory in use they must be less than 0.02 cm. thick, preferably less than 0.01 cm. thick, and although they can be up to 1 cm. square, they are normally about 0.4 cm. square.

It is an object of the present invention to provide a detergent flake that can be formed such that it is less than 0.02 cm. thick, preferably less than 0.01 cm. thick, and is translucent and non-brittle.

Hitherto, it has been proposed, for instance in US. Pat. No. 3,332,880, to utilise alpha-olefin sulphonates as detergent active agents in fabric-washing detergent compositions, it being suggested that these compositions can be prepared in any of the common physical forms associated with fabric-washing detergent compositions, including flakes.

It has now been discovered that, in order to utilise alpha-olefin sulphonates successfully in a detergent flake, then such a detergent flake must contain at least 70% by weight of an alpha-olefin sulphonate and must also contain between 5 and 11% by weight of water. Hitherto it has not been appreciated that the water content of a detergent flake can have such an important influence on the physical properties of the flake. A detergent flake can now be made that fulfills the object of the invention.

The term alpha-olefin sulphonate is herein understood to mean the mixture of anionic detergent active agents obtained when the products of the sulphonation of ice alpha-olefins are neutralised and hydrolysed completely or almost completely.

A detergent flake according to the invention consists essentially of:

(a) From 70 to 95% by weight of an alkali-metal C C alpha-olefin sulphonate;

(b) From 5 to 11% by weight of water;

(0) From 0 to 25% by weight of soap;

=(d) From-0 to 15% by weight of an inorganic detergency builder, selected from the group consisting of sodium silicate, sodium metasilicate, sodium tripolyphosphate, sodium pyrophosphate, trisodium orthophosphatfe', sodium hexametaphosphate, sodium carbonate and sodium bicarbonate;

(e) From 0 to 25% by weight of an organic detergency builder selected from the group consisting of sodium nitrilotriacetate, sodium ethylene diamine tetraacetate, and polyelectrolytes and their partial or total alkali-metal salts; and

(f) From 0 to 25 by weight of a non-soap detergent active agent, other than an olefin sulphonate, selected from the group consisting of anionic, nonionic, cationic and zwitterionic detergent active agents.

The alpha-olefin sulphonates suitable for use in flakes according to the invention are derived from the sulphonation of C -C alpha-olefins. Preferably, the olefins should contain between 12 and 20 carbon atoms, 'and particularly preferably from 14 to 16 carbon atoms. The olefin should preferably consist almost entirely of mono-uns-atunated straight-chain alpha-olefins. Commercially-obtainable supplies of alpha-olefins are generally derived from the cracked-wax process, in which the olefins are extracted from a cracked par-aifin distillate, or by the Ziegler process, in which the olefins are synthesized by polymerisation of a low molecular weight unsaturated hydrocarbon, such as ethylene, with the aid of a Ziegler or similar catalyst. Alternatively, olefins may be prepared by the dehydration of primary alcohols formed, for example, by hyldrogenating esters of naturally-occurring fatty acids such as those derived by the saponification of animal and vegetable oils and fats, or olefins may be prepared by the dehydrogenation of paraflins, although this latter process is not preferred. Preferably, olefin sulphonates derived from Ziegler olefins should be used for the purposes of this invention, as Ziegler olefins usually comprise about 90% by weight of alphaolefins and contain only an insignificant amount of branched-chain material. However, cracked-wax olefins are also suitable, as these generally contain between and by weight of alpha-olefins together with minor amounts of internal olefins and diolefins. The olefins used to prepare the olefin sulphonates for use in the invention should contain as high a proportion of linear alpha-olefins as possible, and if supplies of alpha-olefin were available at present, these would be ideal. However, present technology is unable to produce such material. The man skilled in the sulphonation art is familiar with this problem, and the use of the expression alpha-olefin sulphonate will be understood by him to mean that the material being discussed is derived from olefinic material substantially all of which consists of alpha-olefins, such as cracked wax or Ziegler olefins. Hence, it will be appreciated that throughout this specification the term alphaolefin sulphonate is used to describe the mixtures of olefin sulphonates derived from the sulphonation of commercially available supplies of alpha-olefins,

Alpha-olefin sulphonates are mixtures of various compounds, including various hydroxyalkane sulphonates as well as disulphonates and a major proportion of alkene sulphonate. The proportion of Z-hydroxylalkane sulphonate in the mixture should be kept as low as possible,

preferably to less than 5 percent by weight of the mixture. In contrast, it is often preferable to keep the proportion of 3-hydroxyalkane sulphonate as high as possible, preferably above 20 percent by weight of the mixture, and even more preferably above 30 percent by weight of the mixture. A detailed description of the types and amounts of the vari ous ingredients commonly encountered in alpha-olefin sulphonate is given in US. Pat. No. 3,332,880.

Although in general the alpha-olefin sulphonate will be derived, as explained above, from alpha-olefins, it will be appreciated that when alpha-olefins are allowed to stand in the presence of acidic products, as they will do in batch sulphonation processes, some isomerisation will occur and olefins in which the double bond is not terminal will be formed. It will be appreciated that products containing minor proportions of olefin sulphonates derived from non-terminal double bond olefins are still Within the scope of this invention.

The olefin can be sulphonated in many different ways, such as in stirred-tank reactors or in falling-film reactors. The preferred sulphonating agent is a sulphur trioxide/ air mixture, although other agents, such as oleum, can be used.

The alpha-olefin sulphonate is preferably a sodium salt, although potassium and lithium salts can be used if desired.

In addition to the alpha-olefin sulphonate and water that together make up the essential ingredients of a de tergent flake according to the invention, a flake according to the invention can, if desired, contain up to 25% by weight of one or more additional ingredients. Ideally, these additional ingredients should not comprise more than about by weight of the flake, and particularly preferably they should constitute not more than about 5% by weight of the flake. These additional ingredients can be, for instance, soaps, non-soap detergent active agents other than alpha-olefin sulphonates, detergency builders, perfumes, colourants, enzymes, germicides, fluorescers and antiredeposition agents.

The soaps that can be incorporated into a detergent flake according to the invention can be any of the watersoluble soaps commonly employed in the detergent composition art. Such soaps are alkali-metal salts of longchain fatty acids, the fatty acids being derived either from the saponification of natural fats or oils, or by synthetic means. The sodium salts of such acids are generally preferred, although potassium and lithium salts can be used if desired. The alkyl chain length of the fatty acids will generally be in the range of from 8 to 22 carbon atoms. Examples of natural fats and oils from which such fatty acids can be derived are tallows, coconut oil, palm kernel oil, groundnut oil, tall oil and palm oil. Soaps derived from such natural sources are made up of complex mixtures of fatty acids of differing chain lengths. Examples of these acids are lauric, myristic, oleic, palmitic, capric, caprylic and stearic acids. Synthetic fatty acids will also generally comprise mixtures of these and other fatty acids. Soaps derived from one single fatty acid could be used if desired, but for economic reasons it will generally be preferable to use one of the more readily obtainable natural or synthetic mixtures. The use of distilled fatty acids, whether natural or synthetic, is particularly preferred.

A detergent flake according to the invention can comprise up to 25 by weight of non-soap detergent active agents in addition to the essential olefin sulphonate. Such other detergent active agents can be any of the anionic, nonionic, cationic and zwitterionic detergent active agents commonly employed in the detergent composition art. Examples of these are:

(a) Anionic detergent active agents: alkali-metal salts of organic sulphuric reaction products having in their molecular structure an alkyl radical containing from about 8 to about 22 carbon atoms and a radical selected from the group consisting of sulphonic acid and sulphuric acid ester radicals (included in the term alkyl is the alkyl portion of higher acyl radicals) such as sodium or potassium alkyl sulphates, preferably those obtained by sulphating the higher alcohols (Cy-C13 carbon atoms) produced by reducing the glycerides of tallow or coconut oil; sodium or potassium alkyl benzene-sulphonates in which the alkyl group contains from about 9 to about 20 carbon atoms and in which the alkyl group is attached to the benzene ringe in either the 1 position or at the secondary positions, such as in sodium linear alkyl (C C secondary benzene sulphonate, 2-phenyl-dodecanesulphonate, 2-phenyl-octadecanesulphonate and 3-phenyldodecanesulphonate; sodium alkyl glyceryl ether sulphonates, especially those ethers of the higher alcohols derived from tallow coconut oil and synthetic alcohols derived from petroleum; sodium coconut oil fatty acid monoglyceride sulphates and sulphonates; sodium or potassium salts of sulphur acid esters of the reaction product of one mole of a higher fatty alcohol (e.g. tallow or coconut oil alcohols) and about 1 to 6 moles of ethylene oxide per molecule and in which the alkyl radicals contain about 9 to about 18 carbon atoms; the reaction product of fatty acids esterified with isethionic acid and neutralised with sodium hydroxide where, for example, the fatty acids are derived from coconut oil; sodium or potassium salts of fatty acid amides of methyl taurine in which the fatty acids, for example, are derived from coconut; and others known in the art.

(b) Nonionic synthetic detergent active agents: compounds formed by condensing ethylene oxide with an hydrophobic base formed by the condensation of propylene oxide with propylene glycol; the polyethylene oxide condensates of alkyl-phenols, e.g. the condensation products of alkyl-phenols having an alkyl group containing from about 6 to 12 carbon atoms in either a straight chain or branched chain configuration, with ethylene oxide, the said ethylene oxide being present in amounts equal of 5 to 25 moles of ethylene oxide per mole of alkylphenols (the alkyl substituent in such compounds may be derived from polymerised propylene, diisobutylene, octene, dodecene, or nonene, for example); those derived from the condensation of ethylene oxide with the product resulting from the reaction of propylene oxide and ethylenediamine, such as compounds containing from about 40% to about polyoxyethylene by weight and having a molecular weight of from about 5,000 to about 11,000 resulting from the reaction of ethylene oxide groups with a hydrophobic base constituted of the reaction product of ethylene diamine and excess propylene oxide, said hydrophobic base having a molecular weight of the order of 2,500 to 3,000; the condensation product of aliphatic alcohols having from 8 to 18 carbon atoms, in either straight chain or branched chain configuration, with ethylene oxide, e.g. a coconut alcohol-ethylene oxide condensate having from 6 to 30 moles of ethylene oxide per mole of coconut alcohol, the coconut alcohol fraction having from 10 to 14 carbon atoms; long chain tertiary amine oxides corresponding to the following general formula, R R R N O, wherein R is an alkyl radical of from about 8 to 18 carbon atoms and R and R are each methyl, ethyl or hydroxy ethyl radicals, such as dimethyldodecylamine oxide, dimethyloctylamine oxide, dimethyldecylamine oxide, dimethyltetradecylamine oxide and dimethylhexadecylamine oxide, N-bis(hydroxyethyl)dodecylamine oxide; long chain tertiary phosphine oxides corresponding to the following formula RR'RP 0 wherein R is an alkyl, alkenyl or monohydroxyalkyl radical ranging from 10 to 18 carbon atoms in chain length and R' and R are each alkyl or monohydroxyalkyl groups containing from 1 to 3 carbon atoms, such as dimethyldodecylphosphine oxide, dimethyltetradecylphosphine oxide, ethylmethyltetradecylphosphine oxide, cetyldimethylphosphine oxide, dimethylstearylphosphine oxide, cetylethylpropylphosphine oxide, diethyldodecylphosphine oxide diethyltetradeeylphosphine oxide, bis

(hydroxymethyl) dodecylphosphine oxide, bis (2-hydvoxyethyl) dodecylphosphine oxide, 2 hydroxypropylmethyltetradecylphosphine oxide, dimethyloleylphosphine oxide, and dimethyl-2-hydroxydodecylphosphine oxide; and dialkyl sulphoxides corresponding to the following formula, RRS- 0, wherein R is an alkyl, alkenyl, betaor gamma-monohydroxyalkyl radical or an alkyl or beta or gamma-monohydroxyalkyl radical containing one or two other oxygen atoms in the chain, the R groups ranging from to 18 carbon atoms in chain length, and wherein R is methyl, ethyl or alkylol; such as dodecyl methyl sulphoxide, tetradecyl methyl iSlllPhOXldC, 3-hydroxytridecyl methyl sulphoxide, Z-hydroxydodecyl methyl sulphoxide, 3-hydroxy-4-decyloxybutyl methyl sulphoxide, 3-hydroxy-4-dodecyloxybutyl methyl sulphoxide, 2- hydroxy-B-decyloxypropyl methyl sulphoxide, Z-hydroxy- B-dodecyloxypropyl methyl sulphoxide, dodecyl ethyl sulphoxide, 2-hydroxydodecyl ethyl sulphoxide, dodecyl- Z-hydroxy ethyl sulphoxide.

(c) Ampholytic synthetic detergent active agents which are derivatives of aliphatic secondary and tertiary amines, in which the aliphatic radical may be straight chain or branched and wherein one of the aliphatic substituents contains from about 8 to 18 carbon atoms and one contains an anionic water solubilizing group, such as sodium- 3 dodecylaminopropionate, sodium-3-dodecylaminopropanesulphonate and sodium N-2-hydroxydodecyl-N-methyl-taurate.

(d) Zwitterionic synthetic detergent active agents, namely derivatives of aliphatic quaternary ammonium compounds, sulphonium compounds and phosphonium compounds in which the aliphatic radical may be straight chain or branched and wherein one of the aliphatic substituents contains from about 8 to 18 carbon atoms and one contains an anionic water solubilizing group, such as 3 (N,N-dimethyl-N-hexadecylammonio) propane-l-sulphonate, 3 (N,N dimethyl-N-hexadecylammonia)-2-hydroxypropane-l-sulphonate, 3-(dodecylmethylsulphonium) propane sulphonate, and 3 cetylmethylphosphonium) ethane sulphonate.

Further examples of non-soap detergent active agents commonly used in the art are given in Surface Active Agents, volume 1, by Schwartz and Perry (Interscience 1949) and Surface Active Agents, volume 2, by Schwartz, Perry and Berch (Interscience 1958).

A detergent flake according to the invention can contain one or more detergency builders if this is desired. Such detergency builders can be either inorganic or organic in nature.

Examples of inorganic detergency builders that can be employed are sodium silicate, sodium metasilicate, sodium carbonate, sodium bicarbonate, sodium tripolyphosphate, trisodium orthophosphate, sodium pyrophosphate and sodium hexametaphosphate.

Examples of organic detergency builders that can be used are sodium and potassium nitrilotriacetate, sodium and potassium ethylene diamine tetraacetate and polyelectrolytes, i.e. polycarboxylic acids derived from the polymerization of unsaturated carboxylic acids and unsaturated carboxylic acid anhydrides, such as maleic acid, acrylic acid, itaconic acid, methacrylic acid, crotonic acid and aconitic acid and the anhydrides of these acids, and also from the copolymerisation of the above acids and anhydrides with minor amounts of other monomers, such as vinyl chloride, vinyl acetate, methyl methacrylate, methyl acrylate and styrene. Each of the above acids and anhydrides can also be made to copolymerise with a minor amount of one of the other acids and anhydrides named above. These polyelectrolyte detergency builders are generally incorporated in detergent compositions as their alkali-metal salts. Their sodium salts are preferred, although their potassium salts can also be used.

The production of a detergent flake consisting essentially of wholly-organic ingredients is easier than that of a detergent flake containing inorganic ingredients. This advantage is particularly noticeable in a flake built with trisodium nitrilotriacetate. Therefore, a particularly preferred aspect of the invention is a detergent flake containing up to 25%, preferably about 15%, by weight of trisodium nitrilotriacetate.

In general, for solid components of the flake, it has been found that the more organic and less crystalline is a component, the more acceptable it is in the flake, and therefore a higher proportion of that component can be incorporated into the flake. Thus a flake in accordance with the invention can contain up up 25% of organic, relatively non-crystalline components in addition to the alpha-olefin sulphonate, but a flake can contain no more than about 15% of inorganic crystalline components. Hence, if a flake according to the invention is built entirely with inorganic detergency builders, such as those named above, then an upper limit of about 15% by weight is imposed on the amount of inorganic builder that can be incorporated into the flake.

The detergent flakes according to the invention have been found to have outstanding physical properties and excellent lathering and detergency properties. The good lathering properties of these flakes is particularly noticeable when they are compared with conventional soap flakes, especially if the flakes are used in hard water at low concentrations. Exceptionally good lathering properties are obtained from flakes containing a C -C alpha-ole fin sulphonate. Wash liquor containing detergent flakes of the invention is also found to be exceedingly mild.

It has also been noticed that when conventional soap is used in a bath or basin in which flakes according to the invention are also used, then scum formation in the wash liquor is reduced.

The following examples illustrate the ease of production and the excellent physical and performance properties of detergent flakes according to the invention.

EXAMPLE I 100 g. batches of drum-dried sodium alpha-olefin sulphonate (C -C were mixed with different weights of water and then were milled into diamond flakes on a bench-scale mill with rolls 20 cm. long and 7.5 cm. diameter. Observations were made on the relative ease with which the mix could be flaked and on the physical characteristics (stickiness, appearance) of the flakes.

The results are shown in Table I below:

TABLE I Moisture content EXAMPLE III 100 g. portions of mixtures of sodium alpha-olefin sulphouate (C -C and trisodium nitrilotriacetate (NTA) were moistened with various amounts of water and then converted to flakes on a bench-scale unit with three rolls 20 cm. long and 7.5 cm. diameter. Parts are by weight.

Tests were made with two different mixtures (i) 90 parts alpha-olefin sulphonate, 10 parts NTA (ii) parts alpha-olefin sulphonate, 15 parts NTA The results are given in Tables II and III.

7 TABLE 11 Alpha-olefin sulphonate (90 parts) with NTA parts) Percent moisture content milled Description of flakes: flake by analysis Mix too dry to flake 3.0 Very dry flake 3.5 Do 4.1 Poor flake-too dry 4.4 Good flake 6.6 Very good flake 6.8 Do 8.8 Rather tacky flake 9.4 Reasonable but damp flake 10.7 Damp, tacky flake 12.9 Poor flake 14.8

TABLE III Alpha-olefin sulphonate (85 parts) with NTA parts) EXAMPLE HI Detergent flakes were prepared, where possible, from the compositions shown in Table IV, percentages are given by weight.

TABLE IV In general in this experiment to produce the flakes the dried raw materials are first mixed thoroughly and the mixture then sprayed with the required amount of water. The moistened mass is then milled to homogenise it and finally converted to flake form on conventional flaking equipment such as is used for making soap flakes. Fluorescers, pigments and perfumes can he incorporated without difliculty during the mixing stage.

The flakes obtained from compositions 1 to 7 are Wellformed, are relatively non-brittle and have a satisfactory degree of surface-lustre. These compositions could be milled to a thickness of 0.005 to 0.0075 cms.

The flakes formed from compositions 8 to 19 can only be milled to a thickness of 0.0125 to 0.015 cms. and are brittle and have a poor appearance and lustre.

Although compositions 20 and 21, which contain sodium nitrilotriacetate instead of sodium tripolyphosphate, can be milled to a thickness of 0.005 to 0.0075 cms. the

flakes obtained are also brittle and have a poor appearance and lustre.

The addition of coconut ethanolamide, compositions 12 to 15, or coconut amide, composition 10, even at a 5% level had very little effect.

EXAMPLE IV Flakes prepared from the compositions 1 to 16, 20 and 21, given in Table IV were compared for rate of solution with a soap flake and a non-soap detergent powder.

The soap flake had the following formulation:

Percent by Weight Anhydrous sodium soap* 97 Moisture, fluorescers and preservative 3 Based on a fat charge 25% nut oils, soft oils and 25% tallow.

The non-soap detergent powder had the following formulation:

Percent by weight Suflicient product to give a 0.3% concentration was added to 0 H. water at 30 C. and 40 C. and the liquor swirled by hand. The results are shown in Table V.

Sodium alpha-olefin sulphonate (C1li c1B)---- Sodium tallow alcohol sulphate. Sodium dodecylbenzene snlnh ate Sodium alkane sulphonate ivOw.

Coconut Igepon A 50/60 tallow/coconut a-sulpholatty avid Sodium snlph 1m Sodium tripolyphosphate Trisodium nitrilotrimmm Coconut ethannlnmida Coconut amide- Coconut fatty acids Stearic arid Sodium toluene sulphonate-.. Sodium car Sodium bicarb n Sodium chloride- Sodium per Sodium metasilieate. Anhydrous sodium soap- Sodium carboxymethylcelln Anhydrous alkaline sodium silicate Fluorescers, Perfume, Water 8 8 8 8 8 QOSHN) TABLEV and 0.4% concentration. The mean lather scores are assessed as follows:

A isual assessment is made of the lather generated in a reciprocating paddle machine after times of:

5 30 seconds 1 minute At 30 C. after swirling At 40 C. after swirling 11/; i t

Once Twice fitimes Once Twice 6 times 2 minutes 10 4 minutes 4=maiorlty undissolved 3=eonsiderable amount undlssolved 2=1n ederate amount undlssolved 1=shght amount undissolved i -traoe amount undissolved all dissolved Key:

Composition:

S Ct I 40554.2. I8 09 e BI t d h w a animus m m hn m 1 nC1ol H I n A 4 444 4 m 0 TT f 0 cm W H SS 80 .m u nrw mr w 0 .m M n Md .W m n g fl ww 1 1m 4 h gt. e mn an b 1 X Ca C S m w 0 m V. 2 4.03513 5 m W56 Mm 1 1 in 3 a e x mm S tm m m annnmnenmnmumnmnnnma mm m M a J w M 1 e f. m D D. 6 n t f t e 1 .1 Sande Q a n ne n m D mm 6... a an .1... amv m htra mm d m m m 1. 1 a 80 t t n 0 0 6 W m m 1 836807 .BW. .N. W s s a r m 0 mm 1 w w wnmnwmmmmnnmnmmmnmmm ww mm n m m .m .m. m t 4m t .1 c e r de 1 n n mmb x mm d m m m .I IV e d V a n 0.9 0 e E StO r r M e rs e an mm e E e e et a P 2p n t d L t d V E M 0 80 @0 e 8 maw H m IVa S mi e In m 801 et L n t 0 .1. t m on ma. U I 6 i f n am? m e wa ew N n m m P at r 6 6 a m t we T mam s w m am w w m n v I u e w an? a 1 and Maw a E Tim .w n ,J a a a a m wmw a g A! 2t m f r. W. re S a s va m mm m m R a 2 m P m wmfl .1 n wcq. ssdwm N w mR e w r 4 e umrmsd n m e H a m g rm r ml mmmm m mm m mpnnmo ss t u n eewem emavma mi m t a he .m ddl wMt S W I I. d tr. t e cm e a n 60D UB m O T M SM .mi en 6 k z enh 6 H 06 e t 0 m a ri h accme .1 h g I D. n .b Tt h .1 C mum T 3; mm m wwm mmm T m m 681 234 wk 0 wwm mm w an cw 5 0 5 0 5 0 F0 2 3 3 4 4 5 5 m 1.0..00 96?. 5?- m .m a a m w u u L dm mw wm f u u "n n 3 e n m a M w h m 00000004432331 .20 22 1 a 6 t a v. zw nw m m m nmnnmwnnva m nunanmw mmmwdmh m m m m m m 1 mm txbe n m nnnnnvva ui n n m w m H 3 Y in 0 rm r 1 .l W M M S flnee f t 1100 v mmwmaumm m m wnnnnwmwnnnwnxfinwn I m mmnn i am 1 m .2 m n rw m i w vm. 0 DL; uokae SW10; m m H 00000VM04442442"11121 m WM .hkWiS B e e 3 n 1: 0c tnHTboane M Zen nw m m n n mut d4m nm m m %%11%H-14444443033322 E O W m mfau I. e n u n V k .mo mh m .a dwem mme .f aw mew w mwfwm m m m n I n LQmm 1- a m mm PW m m m h miasisazaamnmnnmwmn 6 .1 a e r. aS u L Tw u em w fimN P w a tn "0 8 Sn t 71 3 1 u n I kw eins r 2 e s T Ie 12 4 s nmm nmzn k 123456789111B1EIW$PD .i 6 0 M. mm w a m tuw m SN man 1308 TABLE VIII Lather scores Soap base (C20) 10) 10) 14) 12) 0.1 percent.

0.3 percent. 24 H. water:

0.1 percent- 0.3 percent- Lather scores in the following table are the mean of six separate tests.

4 H. water:

EXAMPLE VI The compositions 1 to 16, 20 and 21, from Table IV were compared with the soap flake and the non-soap detergent powder given in Example IV for lather and cleansing in a paddle washing machine. Seven pound loads of normally-soiled articles including standard test cloths were washed for 10 minutes in 24 H. water at 40 C. 7

What is claimed is:

1. A etergent flake consisting essentially of:

(a) from 70 to 95 percent by weight of an alkali-metal C -C substantially linear alpha-olefin sulphonate, said alkali-metal being selected from the group consisting of sodium, potassium and lithium;

(b) from 5 to 11 percent by weight of water;

(c) from 0 to 25 percent by weight of soap selected from the group consisting of sodium, potassium and lithium soaps;

(d) from 0 to 15 percent by weight of an inorganic detergency builder selected from the group consist ing of sodium silicate, sodium metasilicate, sodium carbonate, sodium bicarbonate, sodium tripolyphosphate, trisodium orthophosphate, sodium pyrophosphate and sodium metaphosphate;

(e) from 0 to 25 percent by weight of an organic detergency builder selected from the group consisting of sodium nitrilotriacetate, potassium nitrilotriacctate, sodium ethylenediaminetetraacetate, potassium ethylenediaminetetraacetate, and sodium and potassium salts of polycarboxylic acids derived from the polymerisation of unsaturated polycarboxylic acids and unsaturated polycarboxylic acid anhydrides selected from the group consisting of maleic acid, acrylic acid, itaconic acid, methacrylic acid, crotonic acid and aconitic acid and the anhydrides of these acids, and from the copolymerisation of said unsaturated polycarboxylic acids and unsaturated polycarboxylic acid anhydrides with monomers selected from the group consisting of vinyl acetate, vinyl chloride, methyl methacrylate, methyl acrylate and styrene; and

(f) from 0 to 25 percent by weight of a detergent active agent, other than an alpha-olefin sulphonate, selected from the group consisting of anionic, nonionic, ampholytic and zwitterionic detergent active agents.

2. A detergent flake according to claim 1 in which said alpha-olefin sulphonate is a sodium salt.

3. A detergent flake according to claim 1 in which said soap is a sodium soap.

4. A detergent flake according to claim 1 in which said alpha-olefin sulphonate is a C -C alpha-olefin sulphonate.

5. A detergent flake according to claim 1 in which said organic detergency builder is trisodium nitrilotriacetate.

6. A detergent flake according to claim 5 in which said alpha-olefin sulphonate is a C -C alpha-olefin sulphonate.

References Cited UNITED STATES PATENTS 3,332,880 7/1967 Kessler et al. 252555 3,345,301 10/1967 Stein et al. 252545 3,346,629 10/ 1967 Broussalian 260-513 3,356,613 12/1967 Gedge HI 252-527 2,619,469 11/1952 Heald 252550 LEON D. ROSDOL, Primary Examiner P. E. WILLIS, Assistant Examiner US. Cl. X.R.