FI61043C - UPPMJUKNINGSKOMPOSITIONER FOER TYGER - Google Patents

Description

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Patent vjieddelat w (51) Kv.lk./Int.CI.JC 11 D 3/30 SUOM I — FI N LAN D (H) Ptt «nttlh» k «mut - Pattntarnöknlng 762968 (22) H» k «mijpllvl - Anseknlngsdag 18 · 10.76 * '(23) Alkupllvt - Glltlghetsdag 18.10.76 (41) Tullut JulklMksI - Bllvlt ofTcmllg 23. Ot. 77

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Patent- och registerstyrelsen An.ökan utlagd oeh utl.ikrlfwn publlcerad 29.01.82 (32) (33) (31) Pyydetty etuoikeus —Begird prloritet 22.10.75

England-England (GB) 1+ 3336/75 Proven-Styrkt (71) Unilever NV, Burgemeester s'Jacobplein 1, Rotterdam, Netherlands-Holland (NL) (72) Ian Roger Kenyon, Wirral, Merseyside, England-England (GB) ) (7 * 0 Leitzinger Oy (5U) Fabric softening compositions - Uppmjukningskompositioner för Tyger The present invention relates to tertiary amine compositions useful as fabric softeners.

In recent years, blends have been sold for home use that are capable of improving the softness of washed fabrics. Usually, such fabric stretching compositions have been in the form of an aqueous solution or dispersion of a compound that softens the fabric. These solutions or dispersions are added to water, where the fabric pieces are rinsed after washing. The complete washing operation consists of a washing cycle in which the fabric is washed with an aqueous solution of a detergent mixture, after which most of the washing solution is removed from the fabric, and a rinsing cycle in which the fabric is rinsed with water to remove any remaining detergent mixture. The rinsing cycle can be repeated before the washed fabric is dried. The need to add a softener mixture during the rinsing cycle can be inconvenient, especially with automatic washing machines that would otherwise perform the entire wash without interruption.

Therefore, an attempt has been made to develop a wash cycle mixture, i. a mixture which is added to the washing cycle and which is capable of softening the fabrics in the presence of washing-active compounds, whereby the fabric can be cleaned and softened simultaneously. This is a difficult problem because the active softener 2 61043 must be able to settle on the fabric against the effect of a detergent designed to remove dirt from the fabric and in an amount sufficient to soften the fabric, but not so large that the appearance of the fabric deteriorates. Nor should the active softener reduce the detergent activity of the detergent active compound in the mixture. In addition, most compounds known to be fabric softeners are cationic and form insoluble addition products with conventional anionic detergent active compounds. This problem has been proposed to be solved by using certain betaines as softeners, the charge of which is reversed as the pH changes from the temporal conditions of the washing solution where they are anionic to the less temporal conditions of the rinsing solution where they are cationic and their deposition on the fabric is improved. Such betaine is soluble in the washing solution and a small portion of the filled amount remaining in the washing solution residue included in the first rinsing cycle must be sufficient for softening.

German patent 722,281 proposes the use of water-insoluble primary, secondary and tertiary fatty amines in connection with detergents and inorganic salts as textile softeners. The only tertiary amine specifically mentioned is dimethyldodecylamine. British Patent 1,052,847 discloses the use of solid fabric softeners in the wash cycle which are complexes of urea and primary, secondary and tertiary amines having at least one straight chain organic radical of 12 to 18 carbon atoms, but do not mention any specific tertiary amines.

It has now been found that a small group of tertiary fatty amines have particular advantages as fabric softeners for use in the wash cycle because, like the betaines referenced above and unlike dimethyldodecylamine and tertiary and other fatty amines in general, they are negatively charged therefore complexed with anionic detergent compounds but protonate and are thus cationic and fabric-substituting under neutral or slightly achalic conditions under the rinsing cycle. They can therefore be added to an alkaline detergent solution without reducing its cleaning capacity, and since they are insoluble in the washing solution when removed, most of the amine 6104 3 remains in the fabric, making it available for softening when rinsed: This remaining amine becomes native to the fabric , when rinsing water is added, so that it adheres to the fabric before removing the rinsing solution.

The isoelectric point of such an amine is within very narrow limits.

A change in its electronic properties or a reversal of charge must take place between the pH of the washing solution and the pH of the first rinsing solution, which is still weakly alkaline due to the remaining washing solution. The pH of a washing solution containing anionic detergent compounds is generally between 8.0 and 9.9, depending on the detergent builder used. It has been found that when the isoelectric point of the amine is substantially below the pH of the wash solution and at least 0.2 units above the pH of the rinse water, the charge reversal occurs upon addition of the rinse water to the fabric after removal of the wash solution. Amines with the desired properties are tertiary amines having an isoelectric point of 8.3 to 9.8 1 2 and having the structure RR RN, wherein R is an alkyl group having 1 to 6 1 2 carbon atoms, and R and R are substantially straight chain alkyl or alkenyl groups having 10 to 26 carbon atoms.

The isoelectric point of a particular amine can be determined by measuring the electrophoretic mobility of an aqueous amine dispersion under standard concentration and temperature conditions and at different pH values by plotting the mobility against pH to determine the pH of zero mobility. The following table gives the isoelectric scores of some fatty amines. In the table, T and Co denote a mixed alkyl radical derived from hydrogenated tallow acid and coconut oil acid, respectively. From this table it can be seen that those tertiary amines which are members of the above-mentioned special group have the required isoelectric points, while the other amines do not.

T2NH 7.4 T3tf 8.2 T2NCH3 8.8 T2N (CH2) 3CH3 9.0

Co2NCH3 9.1 T2NCH2CH3 9.4 tn (ch3) 2 10.0 TNH2 10.9 4 61 043 The amines in this particular group are generally known compounds and their use has been described for purposes other than fabric softeners. They can be prepared by the methods described in Kirk-Othmer's Encyclopaedia of Chemical Technology, Volume 2, Fatty Amines, or in U.S. Patent 3,471,562, which describes the preparation of dioctadecylmethylamine and its use as an intermediate in the preparation of quaternary ammonium compounds which are themselves cationic. fabric softeners, but whose charge is not capable of reversing. British Patent 1,286,054 and U.S. Patent 3,696,056 describe the use of fatty amines in compositions to control foaming caused by synthetic detergent compositions, but make no mention of fabric softening; the only specifically mentioned tertiary amine having the above structure is a compound termed methyl dihydrated thallamine. The disclosed blends containing this amine do not cause fabric softening. In order to make the present invention useful in practice, it has been found essential to formulate fabric softening amines in such a way as to obtain mixtures different from those described in British Patent 1,286,054 and U.S. Patent 3,696,056.

According to the present invention, the fabric softening composition contains a tertiary amine having an isoelectric point of 8.3 to 9.8 and a structure of

12 12 is RR R N, where R is an alkyl group having 1 to 6 carbon atoms, and R and R

are substantially straight chain alkyl or alkenyl groups having from 10 to 26 carbon atoms and a diluent, wherein the diluent is water or a water-soluble non-surfactant salt; and when the diluent is water, the mixture is a liquid and contains 2 to 50% of amine dispersed in 98 to 50% of water based on the total weight of the amine and water, and when the diluent is a water-soluble, non-surfactant salt, the mixture is solid and contains 6, 3 to 90% of amine and 10 to 93.7% of salt by weight of the mixture.

Tertiary amine plasticizers are most preferably compounds in which R has 1 to 4 carbon atoms, and in particular compounds in which R is a methyl group. R is usually a primary alkyl group. Each of the groups R and R in each mass is preferably from 12 to 22 and in particular from 16 to 1 carbon atoms. The term "substantially straight chain alkyl or alkenyl group" refers to a group that is a substantially unbranched primary alkyl or alkenyl group: A case of branching with such minor amounts that it is not sufficient to destroy the long chain plasticizers is not excluded. Mixtures of amines can be used, for example commercial mixtures of compounds in which the alkyl or alkenyl groups are derived from fatty acids from natural fats, for example when coconut and hydrogenated tallow acids are converted to nitriles and these are then hydrogenated and alkylated. Depending on the type of fatty amine used, such mixed amines are hereinafter referred to as "coconut" and "hydrogenated 1 2 tallow" amines. R and R can similarly be derived from 1 2 soybean oil fatty acids. R and R are preferably groups derived from a common source, in which case in a single compound they are the same group and in commercial mixtures of compounds they mean the same individual groups in the same proportion.

Examples of suitable amines that can be used in wash cycle plasticizers include:

Methyldecylamine Methyldicocosamine

Methyldilaurylamine Methyldi (hydrogenated tallow) amine

Methyldimethylstyramine Ethyldilaurylamine

Methyldisethylamine Ethyldiethylamine

Methyldimararylamine Propyldistearylamine

Methyldisearylamine Butyldistearylamine

Methyldiarakidylamine Ethyldiococosamine

Methyldococosylamine Ethyldi (hydrogenated tallow) amine

Methylditetracosylamine Butyldi (hydrogenated tallow) amine

Particularly suitable are methyldicocosamine and methyldi (hydrogenated tallow) amine.

The invention provides a process for preparing an aqueous amine dispersion according to the invention, wherein the amine is dispersed in water in the presence of an emulsifier, preferably at a temperature at which the amine is in liquid form. Suitable emulsifiers are listed in Kirk-Othmer1 in Encyclopaedia of Chemical Technology, Volume 8, pages 128-130. Upon cooling, the resulting emulsion may become a suspension upon solidification of the amine. Most dispersions prepared in this way are short-lived because they are unstable and, if stored before use, tend to separate into an aqueous phase and a solid amine phase: Successful preparation of dispersions that are stable for several weeks has been difficult, it has been observed , that using standard emulsion technology methods to select an emulsification system with an optimal hydrophilic-lipophilic balance (HLB), it is not possible to prepare stable emulsions. However, it has been found that satisfactorily stable dispersions can be prepared by adding an emulsifier having a hydrophobic group similar to the hydrophobic groups of the amine; this seems to work in such a way that it is possible to form amine particles with an anionic polar backbone of the emulsifier on the surface with a negative charge. This alters the effective isoelectric point of the amine, while packaging the hydrophobic group of the emulsifier with the corresponding groups of the amine allows this group to remain within the particles.

The liquid mixture according to the invention thus best contains, as emulsifier, an anionic surfactant having a hydrophobic group which is a substantially straight-chain alkyl or alkenyl group having an average chain length of 2 1/2 of the average content of the amine groups R and R. the length of the chain. Particularly suitable are emulsifiers having a hydrophobic group distribution substantially the same as that of the amine. The anionic end group of the emulsifier may be a carboxylate, sulfate, sulfonate, phosphate or phosphonate. Suitable emulsifiers may be selected from the following: sodium laurate, myristate, palmitate and stearate, disodium hexadecenyl succinate (having an effective hydrophobic chain length of 16 carbon atoms), sodium N-thalloyl glutamate length of 17 carbon atoms), sodium „α-olefin sulphonate (with a hydrophobic chain

Ib lo has an effective length of 17 carbon atoms), sodium tallow fatty sulfonate (having an effective hydrophobic chain length of 17 carbon atoms) and sodium C 1 -C 20 n-alkyl phosphate (having an effective hydrophobic chain length of 18 carbon atoms). Other useful emulsifiers include sodium hexylbenzenesulfonate and sodium octadecylbenzenesulfonate. Instead of sodium salts, a salt of any equivalent cation which causes water solubility can be used, for example lithium, potassium or ammonium.

When the amine used is methyl-dicocosamine, the emulsifier is sodium laurate, and in particular the sodium salt of coconut oil fatty acid. When the amine is a methyldi (hydrogenated tallow) amine, the emulsifier is preferably sodium stearate and especially the sodium salt of hydrogenated tallow acid.

The liquid amine mixture preferably contains from 5 to 30% by weight of amine and in particular from 7 to 25% by weight of the total amine and water, since such concentrations are advantageous in practice because they correspond to the existing methods of liquid fabric treatment agents. that an effective amount of amine is obtained in the washing solution. An effective amount of emulsifier is selected to be between 0.02% and 10% by weight of the dispersion, and dispersionase is generally used in an amount of 0.1% to 20% by weight.

The solid amine mixture preferably contains at least 6.5 and in particular at least 7% amine. The amount of salt present is usually less than 75% by weight of the mixture.

As water-soluble non-surfactant salts, the main washing salts are best used. By "basic detergent salt" as used herein is meant a salt capable of increasing the detergent activity of a detergent active compound. Suitable washable base salts include inorganic builders such as sodium ortho, pyro-, trimethase and tripolyphosphates, sodium carbonate and sodium silicate. Examples of organic building materials are salts of organic acids such as sodium citrate, sodium oxide acetate, sodium carboxymethyloxysuccinate, sodium nitrilotriacetate and sodium ethylenediamine tetraacetate.

Non-surfactant salts other than detergent builders useful in the solid compositions of the invention include sodium perborate or percarbonate, which have the ability to bleach, and sodium sulfate.

When the mixture contains a detergent base salt, it preferably also contains an anionic detergent compound, especially a non-soap (or synthetic) anionic detergent compound. Such a mixture preferably contains 6.5 to 35% of an amine, 3 to 60% of an anionic detergent active compound and 5 to 75% of a detergent base salt by weight of the mixture.

8 61043

When the composition of the invention contains an anionic detergent active compound, it may be a water-soluble or water-dispersible alkali metal salt of an organic acid, especially a sodium or potassium salt, or a corresponding ammonium salt or a substituted ammonium salt. Examples of suitable organic acids are alkylbenzenesulfonic acids whose alkyl groups contain from 8 to 20 carbon atoms, for example straight-chain C 1-5 alkylbenzenesulfonic acids; alkyl and alkenyl sulfonic acids having from 8 to 22 carbon atoms, for example compounds known as olefin sulfonates which can be obtained by reacting sulfur trioxide with straight-chain and branched olefins, in particular "cracking wax" or "Ziegler" alpha-olefins, or by reacting compounds obtained by reacting with sulfur dioxide and chlorine followed by hydrolysis or reaction of the olefins with bisulfites; alkyl sulfiosuccinates obtained by reacting maleic acid esters with bisulfites; Alkyl sulfuric acids having 8 to 22 carbon atoms obtained by reacting alcohols with sulfur trioxide; alkyl ether sulfuric acids obtained by reacting 1 mole of alcohols having 6 to 18 carbon atoms with 1 to 15 moles of ethylene oxide or mixtures of ethylene oxide and propylene oxide and then reacting the condensation product with sulfur trioxide; Naturally occurring or synthetic aliphatic carboxylic acids having 10 to 22 carbon atoms, in particular soaps obtained by decomposing triglyceride oils; and N-acylated isethionic and sarcosic acids in which the acyl groups are derived from such aliphatic carboxylic acids. Other suitable anionic detergent active compounds are described in Schwarz and Perry, "Surface Active Agents", volume I, and Schwarz and Perry, "Surface Active Agents and Detergents", volume II.

The compositions of the invention may contain other ingredients of fabric detergent compositions, for example foaming agents such as coconut monoethanolamide; antifoaming agents; chlorine-releasing bleaches, for example trichloroisocyanuric acid and sodium and potassium dichloroisocyanurates; anti-redeposition agents such as sodium carboxymethylcellulose; and perfumes, dyes, fluorescent agents, corrosion inhibitors, termicides and enzymes.

The invention provides a process for preparing a solid mixture according to the invention, in which the amine is mixed with a non-surfactant salt and, if present, an anionic detergent active compound and, if necessary, the mixture is granulated. The solid mixture is best prepared as a spray-dried powder. Such a powder can be obtained by preparing an aqueous slurry containing the ingredients of the mixture and heating the slurry to 80 ° C, at which temperature the amine is liquid, and can be uniformly dispersed with slurry into a slurry which is then spray dried to a powder containing a uniformly distributed amine.

For household use, the liquid mixture according to the invention can be added in small amounts sufficient for softening, for example from a bottle or a closed small bag, for example 10-100 ml, to a cloth in a washing machine together with a suitable detergent mixture, for example washing powder. The solid compositions of the invention which do not contain the detergent required for washing are added in the same manner, and the solid compositions containing the detergent active compound required for washing are used in the same manner as normal detergent compositions. To achieve good results, the pH of the wash solution should be at least 0.2 pH units above the isoelectric shaker of the amine used. This can be achieved by selecting the appropriate amine for a particular wash solution or by adjusting the alkali content of the wash solution as needed. The pH of the washing solution is preferably below 9.8 to avoid an excessive buffering effect and to reduce the pH of the rinsing solution as necessary without lowering the pH of the natural rinsing water: However, a high pH washing solution may be diluted with water after washing and before removal. if it is desired to reduce the proportion of residual washing solution in the alkalinity of the first rinsing solution. For practical reasons, the pH of the washing solution must be above 8.5 to allow the use of an amine with an isoelectric point at least 0.2 units above the pH of the first rinsing solution.

The invention also encompasses a fabric softening method in which an aqueous anionic wash solution having a pH above the amine isoelectric point is prepared from the composition of the invention, the fabric is washed with a wash solution and the pH of the wash solution in contact with the washed fabric is then lowered below the amine isoelectric point. Most of the washing solution present during the washing step is preferably separated from the washed fabric and the pH reduction is performed by adding rinsing water to the fabric containing the remaining washing solution.

61043 10

The invention also comprises a softened fabric containing 0.0005 to 0.01 and most preferably 0.001 to 0.005 parts by weight of a tertiary amine belonging to the special group defined above as a surface coating.

The invention is illustrated by the following examples in which all temperatures are in degrees Celsius.

Example 1 To an 80 degree solution of sodium laurate (0.15 g) in water (84.85 g) was added molten methyldicocosamine (15 g) and the mixture was stirred and ultrasonically dispersed until homogeneous.

The front automatic tumble washer was loaded with soiled laundry (2.7 kg) and 16 pieces (side length 20.3 cm) of clean cotton towel followed by 50 degree water (2o liters), amine dispersion (75 ml) and detergent product (100 g), having a composition by weight of:

Sodium dodecylbenzenesulphonate 7.5

Condensate of tallow fatty acid amine with 11 molar equivalents of ethylene oxide 3.5

Cured Tin Sodium Soap 1.0

Sodium tripolyphosphate 64.9

Alkaline sodium silicate 1.0

Sodium sulphate 9.5

Sodium carboxymethylcellulose 1.0

Sodium chloride 1.4

Fluorescent 0.2

Water 10

The liquid: garment ratio of the obtained batch was 7: 1 and the pH of the aqueous solution was 9.3. The fabrics were washed using a standard program in which the batch was heated to 95 ° C with drum stirring for 35 minutes and then wetted to leave approximately 20% wash solution and rinsed four times with cold water (20 liters, pH 7.5, giving the first rinse solution). pH 8.7), centrifuged after the third and fourth rinses.

The fabric was then allowed to dry in the atmosphere. The dried fabric 11 61043 contained about 0.002 parts of amine by weight as a surface coating.

A similar procedure was performed without the amine dispersion. The garments were assembled in pairs, one washed with amine and the other without. An evaluation team of five users directly compared the pairs, indicating for each pair which he considered softer.

Of the 80 pairwise comparisons, in 77 cases a softer treated with an amine dispersion was selected as softer.

Example 2

An amine dispersion was prepared according to Example 1, but methyl di (hydrogenated tallow) amine was used as the amine and sodium teaate as the emulsifier.

The paddle washing maschine was loaded with soiled laundry (2.7 kg) and 16 pieces (side length 20.3 cm) of cotton towel followed by 50 degree water (68 liters), amine dispersion (50 ml) and detergent product. (100 g) having the following composition by weight:

Sodium dodecylbenzenesulphonate 6.0

Condensate of hardened tallow alcohol 18 molar equivalents with valent ethylene oxide 4.0

Cured Tin Sodium Soap 8.0

Sodium tripolyphosphate 33.0

Alkaline sodium silicate 8.0

Sodium sulphate 3.1

Sodium carboxymethylcellulose 1.0

Sodium perborate 25.0

Fluorescent agent and perfume 0.7

Water 11.2

The resulting charge had a liquid: fabric ratio of 25: 1 and a wash solution pH of 9.7. The fabrics were washed on a standard program in which, with shaking, the batch was heated to 95 ° C for 40 minutes, drained and excess water removed by centrifugation to leave about 10% washing solution, and rinsed twice with cold water (60 liters, pH 7.5 , whereby the pH of the first rinsing solution was 8.2), after the last rinsing, the spin was centrifuged and the fabric was allowed to dry in the atmosphere. The dried fabric contained about 0.0015 parts of amine as a surface coating to the weight of the fabric.

The procedure was repeated using 32 pieces without the amine dispersion: 16 pieces were removed and dried, and the washing machine was placed on one more rinse and spin cycle, 50 ml of a commercial rinse aid containing 6% by weight of dimethyldicocosammonium chloride and dimethylide (hydrogenated tallow) ammonium chloride was added. the remaining 16 pieces were dried.

16 pieces from each treatment were arranged in triplicate and their softness was compared by a 5-member evaluation team. In each of the three groups, it was possible to give 1 point for the softest piece, 2 points for the next softest and 3 points for the coarsest. The total scores were as follows.

Garments treated with amine dispersion 130 with commercial rinse aid 113 detergent 237 only This shows that the softening ability of the amine dispersion used as a softener for the wash cycle was not significantly worse than that of the commercial quaternary ammonium salt mixture used as a softener and rinse aid softener.

Example 3

An amine dispersion was prepared according to Example 1, but methyl distearylamine (isoelectric point 8.7) was used as the amine and sodium stearate as the emulsifier.

A mixture containing the following ingredients by weight was used as the detergent: i3 61 043

Sodium radododecyl benzene sulphonate 14.0

Coconut ethanolamide 2.0

Sodium tripolyphosphate 33.0

Alkaline sodium silicate 6.0

Sodium sulphate 17.0

Sodium carboxymethylcellulose 0.5

Sodium perborate 20.0

Fluorescent agent and perfume 0.2

Water 7.3

Four pieces of clean cotton towel (side length 20.3 cm), water (800 ml), amine dispersion (2 ml) and detergent mixture (3.2 g) were placed in the Tergotometer. The liquid: garment ratio was 20: 1 and the pH of the washing solution was 9.7. The garment was washed for 15 minutes at 80 ° C, the washing solution was removed to leave about 10%, the garment was rinsed twice in cold water (800 ml, 24 ° H, pH 7.5 to give the pH of the first rinsing solution 8.2) and dried. . The dried fabric contained about 0.002 parts of amine by weight as the surface coating.

The procedure was also performed without the use of an amine dispersion. The softness of the fabric groups was tested in pairs as in Example 1. Each member of the evaluation group found the fabric treated with the amine dispersion softer than the fabric treated with detergent alone.

Examples 4 and 5

An amine dispersion (Example 4) was prepared as in Example 2, but the amine used was methyldialkylamine having an isoelectric point of 9.3 and each alkyl group derived from a commercial mixture of C 1-4 and C 22 straight chain saturated fatty acids with C 20 C acid predominant.

For comparison, co-dispersions were prepared using tri (hydrogenated tallow) amine and dimethyl (hydrogenated tallow) amine as amines with isoelectric points of 8.2 and 10.0, respectively. The amine dispersion of Example 2 was also used (Example 5).

14 61 043

Each emulsion followed the washing procedure of Example 3 (pH 9.7 of the wash solution and pH 8.2 of the first rinse solution). The garments were divided into a group of 16, 4 pieces containing a piece washed with each emulsion. A 5-person evaluation team rated their softness by giving 1 point to the softest and 4 points to the roughest egg.

The combined softening points obtained were:

Garments treated with dispersions of the following substances: Methyldi (C20-C22alkyl) amine (Example 4) 136

Methyldi (hydrogenated tallow) amine (Example 5) 167 tri (hydrogenated tallow) amine 301 dimethyl (hydrogenated tallow) amine 196

The scores obtained with the amine dispersions of Examples 4 and 5 are indicative of the softening effect compared to the effect obtained with the other dispersions. The garments washed with the last dispersion had greasy deposits due to the precipitation of the amine and the anionic detergent used.

Example 6

The amine dispersion of Example 2 was used as a wash cycle softener as in Example 3. It was compared to a commercial wash cycle softener containing 14% by weight of quaternary imidazoline methyl sulfate. The procedure used was similar to that of Example 3 except that 1 ml of the amine emulsion of Example 2 and 1 ml of a plasticizer containing the quaternary imidazoline salt were used as softeners for the wash cycle. Washing was also performed using a detergent mixture containing no softener, both with and without the commercial rinse aid of Example 2 (1 ml) added to the last rinse solution. The evaluation teams evaluate the dried garments obtained as above. The softness points obtained were: 15 61 043

Garments treated with a dispersion of methyldi (hydrogenated tallow) amine i 108 with a commercial wash cycle softener 270 with a commercial rinse aid 142 with detergent 280 only

Examples 7-15

Amide dispersions were prepared as in Example 2, but using different amine concentrations, i. 5, 10, 20, 25, 30, 35, 40, 45 and 50% methyldi (hydrogenated tallow) amine by weight of the dispersion and sodium stearate as emulsifier. The emulsions were found to be stable for at least 6 weeks at ambient temperature.

The procedure of Example 3 was fed using the amine dispersion but replacing the amine dispersion with 1 ml of the 30% dispersion shown above (Example 11) to give a softened cotton fabric.

Examples 16 to 20

Amine dispersions were prepared as in Example 2, but using different concentrations of emulsifier, i. 0.015, 0.45, 0.75, 1.5 and 3% sodium stearate by weight of the dispersion. The dispersions were found to be stable for at least 6 weeks at ambient temperature, and the dispersion containing 0.45% emulsifier was stable for at least 6 months.

Examples 21-30

Amine dispersions were prepared as in Example 2, but using various emulsifiers. The stability length of each emulsion at 20 ° C was monitored.

16 61 043

Example Emulsifier Stability 21 Sodium laurate 10 days 22 Sodium myricate 2 weeks 23 Sodium palmitate at least 6 weeks 24 Sodium hexadecenyl succinate at least 10 weeks 25 Sodium N-thaliacylglutamate 4 weeks 26 Sodium Clfi-Cia α-olefin sulfonate 4-enecene weeks 29 Sodium tallow fatty acid sulphonate at least 10 weeks 30 Sodium C 1 -C 10 alkyl phosphate 6 weeks

Examples 31 and 32

Stable amine dispersions were prepared according to Example 1, but methyldicocosamine and sodium salt of coconut oil fatty acid were used as the amine and emulsifier, respectively: and methylide (hydrogenated tallow) amine and hydrogenated tallow fatty acid sodium salt, respectively.

Example 33

A solid fabric softening composition was prepared containing the following ingredients by weight.

Sodium dodecylbenzenesulphonate 14.0

Coconut ethanolamide 2.0

Sodium tripolyphosphate 33.0

Sodium sulphate 6.9

Alkaline sodium silicate 6.0

Methyldi (hydrogenated tallow) amine 10.0

Sodium carboxymethylcellulose 0.5

Fluorescent 0.4

Sodium perborate 20.0

Water 7.2

All ingredients except amine and perborate were mixed with additional water (62 parts) to a slurry, heated to 80 ° C, the amine was added in the molten state and the mixture was mixed well and spray dried to a dry free flowing powder with which 61043 was finally mixed with perborate.

The mixture was washed at a concentration of 0.4% according to Example 3 in a Tergotometer with a pH of 9.7 in the washing solution and a pH of 8.3 in the first rinsing solution. The dried garment contained about 0.004 parts of amine by weight as a surface coating. A control wash was also performed using a similar mixture in which the amine was replaced with the same amount of sodium sulfate. The evaluation team performed the comparison as above and found the amine-treated garment softer in each case.

Example 34

A solid fabric softening mixture was prepared containing the same ingredients as the detergent product of Example 1 except that 7.5 parts of methyl di (hydrogenated tallow) amine was replaced by the same amount of sodium sulfate. The mixture was prepared by mixing together all the ingredients except the amine and a portion of sodium tripolyphosphate (23 parts) together with additional water (60 parts) to a slurry, heating the mixture to 80 ° C, adding the molten amine, mixing the mixture thoroughly and spray drying the mixture into a dry free flowing powder. mixed.

The mixture was washed at 0.2, 0.4 and 0.6% cotton pieces in a Tergotometer according to Example 3, the pH of the washing solution being 9.3 and the pH of the first rinsing solution being 8.1. Comparative washes were also performed using the detergent product of Example 1. The comparison performed by the evaluation team on the previous stage showed that the amine-treated garment was softer than the comparison in all cases.

Example 35

A mixture was prepared according to Example 34, but methyldicocosamine was used as the amine: The mixture was used in a 100 g front-loading automatic washing machine in a similar washing treatment as in Example 1, where the pH of the washing solution was 9.3 and the pH of the first rinsing solution was 8.7. The treatment softened the cotton fabric.

Claims (15)

1. Softening composition for fabrics containing higher alpha-tertiary amine, and as diluent water or water-soluble non-surfactant salt, characterized in that the isoelectric point of the amine is 8.3 - 9.8 and structure RR RN, wherein R is 2 is an alkyl group of 1-6 carbon atoms, and R and R are substantially linear alkyl or alkenyl groups of 10-26 carbon atoms, and where the diluent is water, the composition is liquid and contains 2-50% by weight of amine dispersed in 50% by weight water of the total amount of amine and water, and since the diluent is a water-soluble, non-surfactant site, the composition is solid and contains 6.3-90% amine and 10-93.7% by weight of the composition which may contain a anionic emulsifier. Composition according to claim 1, characterized in that in the group R of the amine there are 1-4 carbon atoms. Composition according to claim 2, characterized in that R is a methyl group. 4. A composition according to any one of the preceding claims, characterized in that in both groups R and R there are 16-18 carbon atoms. Composition according to claim 3, characterized in that the amine is methyldicocosamine or methyldi (hydrogenated tallow) amine. The composition according to any preceding claim, wherein the diluent is water, characterized in that the composition contains 7-25% by weight amine of the total amount of amine and water. Composition according to claim 6, characterized in that it contains as an emulsifier an anjanic surfactant having a hydrophobic group which is a substantially linear alkyl or alkenyl group, whose average chain length is - 2 1/2 carbon atoms of amine groups. R and R average chain length.