SE464139B - CONCENTRATED TEXTILE SOFT COMPOSITION AND PROCEDURES FOR THE MANUFACTURING OF THE SAME - Google Patents

Description

U.S. Pat. No. 3,681,241 discloses a concentrated fabric softening emulsion consisting essentially of 3.5 to 6.5 parts by weight of a compound such as distearyl dimethylammonium chloride, from 3.5 to 6.5 parts by weight of an alkylamidoimidazolinium alkyl sulfate and from 0 to 3 parts by weight of another but similar fatty amido-imidazolinium alkyl sulphate, the latter being said to give the composition stability at low temperatures. The total proportion of active substances is stated to be in the range from approx. 8 to 13%.

British Patent Application 2,053,249, published February 4, 1981, discloses cationic fabric softening compositions containing 15 to 60% by weight of cationic plasticizer, 25 to 75% by weight of aqueous medium and 0.5 to 40% by weight of specified water-soluble polymer.

U.S. Pat. No. 3,974,076 discloses quaternary ammonium-containing emollient compositions having conventional levels of cationic substances, i.e. ca. 3% to approx. 6%. These compositions are characterized in that the substantially water-soluble plasticizing quaternary ammonium compound has a very small particle size, i.e. 90% by weight of the quaternary ammonium compounds are in the form of particles that pass through a 1.2 micron filter. The compositions are described as a combination of the cationic plasticizer, a C8-C20 alkyl alcohol having approx. 0.1% to approx. 2.0% of a nonionic surfactant that has an HLB value of from approx. 8 to approx. 15 and preferably from approx. 10 to approx. The preferred nonionic substances have a lipophilic hydrocarbyl residue corresponding to 9 to 15 carbon atoms and 7 to 13 hydrophilic ethylene oxide residues.

This patent does not address the problem of the stability of aqueous cationic emollient compositions, but rather seeks to improve the level and uniformity of the emollient obtained using conventional concentrations.

Each of U.S. Patents 4,076,632; 4,157,307 and 4,233,164 describe quaternary ammonium compounds as plasticizers which contain protonated ethoxylated amine, but none of these describe salts of the amine and even less salts with high molecular weight organic acids (ie higher fatty acids, eg C12 to C30; alkylarylsulfonic acids (eg C12-C18-alkylbenzenesulfonic acids; C12 to C30 Perrofin (alkyl) sulfonic acids; C12 to C30 olefin sulfonic acids; mono- and diphosphoric acid esters of C8 to C30 alcohols including ethoxylate of these alcohols with from 1 to 100 moles of ethylene oxide). U.S. Patent 4, 118.32? describes conventional levels of cationic substances (0.1 to 10% by weight, preferably 1 to 8% by weight) together with organic phosphate esters, as antistatic agents.

Summary of the Invention The present invention provides concentrated aqueous emollient compositions which are stable at low and high temperatures and which are based on quaternary emollient ammonium compounds and a minor amount of an amine salt of an ethoxylated long chain amine having a long chain organic acid and an electrolyte. Water-soluble polymers such as polyethylene glycol (e.g., having a molecular weight of 400) are a preferred optional ingredient.

Detailed Description of the Invention The compositions of the present invention are stable aqueous compositions containing a high proportion of cationic fabric softener consisting of a water-dispersible quaternary ammonium compound according to the following description, and an amine salt likewise described below.

The aqueous compositions according to the invention contain at least approx. 12% cationic plasticizer but can contain up to approx. 20% of this, which cationic plasticizer has the general formula: in which the R groups are selected from C1 to C30 aliphates, preferably alkyl or alkenyl, aryl (eg phenyl, tolyl, cumyl, etc. ); aralkyl (eg benzyl, phenethyl, etc.); and halogen, amide, hydroxyl and carboxy substituents thereof; with to C and preferably C14 to C18 and the others are lower alkyl and most preferably the restriction that at least one R is C is at least two R C14 to C18 and the others are lower alkyl with C1 to C4 (and is preferably methyl or ethyl) and Y is a water solubilizing anion such as chloride, bromide, iodide, fluoride, sulfate, methosulfate, nitrite, nitrate, phosphate and carboxylate (ie acetate, adipate, pmpyxmate, phthalate, benzoate, oleate, etc.). typical cationic substances of formula I are: distearyl dimethyl ammonium chloride ditallow dimethyl ammonium chloride distearyl dimethyl ammonium bromide dihexadekyldimetylammoniumklorid_ di (hydrogenated tallow) dimethylammonium bromide distearyl di (isopropyl) ammonium chloride distearyldimetylammoniummetosulfat the invention included in the amine salts are based on ethoxy- lated long chain amines and long chain organic acids.

The amines are typically C12 to C30 aliphatic amines and are preferably C12 to C20 amines and mixtures thereof which are controlled by from 1 to about 100 moles of ethylene oxide. The amines can also be reacted with propylene or butylene oxide and then with ethylene oxide. The final oxyalkylated amine should be a water-soluble product. Amines derived from natural fatty acids, such as "Armeens" and "Ethomeensf", are particularly valuable and generally comprise a mixed alkyl within the range C10 to C18, or C12 to C16, or C12 to C15, or C16 to C18 and similar. The preferred ethoxylated amines are those containing from about 5 to approx. 50 moles of condensed ethylene oxide and ethoxylated amines with approx. 10 to approx. 35 moles of condensed ethylene oxide are even more preferred.

Preferably they should contain 12 to 20 moles of ethylene oxide.

The third component is an ionic electrolyte material in an amount of from about 0.1 to approx. 1.5% by weight. The use of an electrolyte not only helps to regulate the viscosity but also helps to stabilize the system against gel formation and phase inversion at high temperatures, e.g. Sodium chioria and calcium chioria are particularly suitable electrolytes. Other suitable electrolytes include sodium formate, sodium nitrite and sodium acetate as well as water-soluble salts of other cations such as potassium, lithium, magnesium ammonium and the like.

Smaller amounts of lower alkanols can be used, especially when it is desired to further modify the viscosity. Alcohols generally tend to lower the viscosity at room temperature, although smaller amounts can lower the phase inversion temperature. The preferred compositions of the invention have the phase inversion temperature which is higher than about 80 ° C and preferably higher than about 90 ° C, the amount of alcohol being in the range of from about 1% to about 10% by weight. Ethyl alcohol and propyl alcohol are particularly suitable alcohols.

In addition to the above-mentioned constituents of the emollient compositions of the invention, numerous conventional additive constituents and optional constituents which do not adversely affect the stability and / or functional properties of the present compositions may also be included therein. Thus, for example, perfumes, dyes, pigments, thickeners, germicides, optical brighteners, anticonvulsants (eg, sodium silicate), water-soluble polymers, antistatic agents and the like may be commonly present. 464 139 6 When included, each of them can be from 0.01% by weight to approx. 5% by weight of the composition.

It is, of course, known that most of the available chemical materials, and especially those containing a hydrocarbyl residue, are generally mixtures of closely related residues. Thus, the long chain alkyl substituents (R) of the cationic substances used in this invention need not only be a single carbon chain but are more likely a mixture. A separate base base, in which the alkyl groups are derived from tallow, may contain approx. 35% G1 Goch 60% C18 and Inner lengths C14 also other. The fabric softening compositions according to the invention and the invention must, in addition to viscosity and phase stability, have the required viscosity (ie for pourability) and water-dispersibility in the rinsing step (or other form of dilution before use), which consumers have come to accept and request based on their use of less concentrated products. The products referred to herein may have viscosities in the range of from about 30 cps to approx. 250 cps and preferably from approx. 40 cps to approx. 120 cps.

In addition to providing excellent dispersing properties in water, the amine salts used herein also contribute to the softening so that, for example, a concentrate consisting of 12% quaternary compound and 2% amine salt is not only equivalent to twice the amount of a conventional 6% cationic composition but is almost 2, 5 times more efficient.

The general procedures for the preparation of the present composition are manifold, with the final product varying somewhat in stability. The chosen method depends on the components used and differs in the order of addition of the materials and the process conditions used.

A typically preferred process (A) involves adding the nonionic material and dyes, if any, to the calculated amount of water having a temperature of about 7,464,139 Approx. 700C. To this solution previously added with amine salt is slowly added the cationic plasticizer in the "molten" state (50-60 ° C). Usually a gel forms.

The mixture is allowed to cool to approx. 40 ° C after which the electrolyte is added to break the gel. The composition is then cooled to room temperature with stirring. A modification of method (A) involves adjusting the pH to approx. 12 before adding the molten cationic material. In this case, no gel is formed. After cooling to approx. 40 ° C, the pH is adjusted again, to 5 or 6, followed by cooling to room temperature with stirring, after which electrolyte is used to adjust the viscosity (method B). Yet another process (C) involves adding nonionic agent and electrolyte to at least 80% hot water (about 40 ° C) and then adding cationic plasticizer and amine salt as in process (A). In general, no gel is formed. Then any remaining water is added and the composition is then cooled with stirring to room temperature.

The following examples are intended to illustrate the invention, but without limiting it. Shares are by weight unless otherwise stated.

Example I In accordance with process (A) described above, 1 part of polyethylene glycol (molecular weight 400) and parts of 1.2% color solution are dissolved in approx. 70 parts water at a temperature of approx. 70 ° C.

To this solution is slowly and with stirring added 17.6 parts of distearyl dimethylammonium chloride (75% active and containing about 10% isopropanol and the remainder water) in molten form and to which previously 3.7 parts of Ethomeen T 25 (tallow amine with 40 % C16 and 60% C18 condensed with moles of ethylene oxide) and 1.3 parts dodecylbenzenesulfonic acid (temperature = 55 ° C). You get a gel. This is cooled to approx. 4000 after which 0.5 parts of calcium chloride dihydrate are added.

The mixture is cooled to room temperature (approx. 20 ° C) with stirring. A stable product is obtained with a viscosity of 464 139 8 of approx. 100 cps.

Example II The procedure of Example I is repeated using the following parts of: (A) cationic agent (active), (B) amine, (C) sulfonic acid and (D) electrolyte. (a) A = 12; B = 1.0; C = 0.32; D = 0.5 (b) A = 14; B = 1.5; C = 0.52; D = 0.5 (c) A = 16; B = 1.8; C = 0.63; D = 0.7 (d) A = 18; B = 2.5; C = 0.88; D = 1.0 Example III Examples I and II are repeated using the following instead of distearyl dimethylammonium chloride: (a) ditallow dimethylammonium chloride (b) distearyl dimethylammonium methosulfate (c) di (hydrogenated tallow) dimethylammonium bromide (d) hexadecyldimethylammonium chloride (e) distearyl diethylammonium chloride Example IV Examples I, II and III are repeated in each case adding some polyethylene glycol (molecular weight 400) together with the amine salt in the first step of the process of the invention.

Polyethylene glycol (molecular weight 400) is an example of low molecular weight water-soluble polymers which, if desired, can be used in the emollient compositions of the invention. With respect to other suitable poemaxes, reference may be made to the aforementioned British patent application 2,053,249 A, the contents of which are incorporated herein by reference. The compositions of the invention may be included in any of these, including other water-soluble polymers. In the compositions according to the invention it is possible to use from 0.1% to 20% by weight of these materials, calculated on the weight of the whole composition.

Example V Each of the following examples I to IV is repeated using as electrolyte one of the following: (a) sodium chloride (b) sodium nitrate (c) sodium formate (d) ammonium bromide (e) potassium chloride (f) calcium nitrate (g) lithium acetate (h) Magnesium chloride Example VI Each of Example IV is repeated, compositionally, but according to procedure (B) to prepare the compositions. In this procedure, the process conditions described in Example I are changed by adjusting the pH to 12 with sodium hydroxide after dissolving the amine salt (and using polyethylene glycol), after which the pH is readjusted to pH 5-6, with hydrochloric acid after addition of the cationic material. At this stage no gel is formed, in contrast to procedure (A). The electrolyte is added after the mixture is cooled to room temperature.

Example VII Each of Examples I-V is repeated again, compositionally, following procedure (C) for preparing the compositions. In this procedure, the amine salt (and water-soluble polyethylene glycol) was dissolved in 80% of the constituent amount of water having a temperature of 35-40 ° C. Then the electrolyte is added, followed by molten cationic material. Then the remaining amount of water is added and the mixture is cooled to room temperature with stirring.

Example VIII Using the aforementioned procedure (A), 1 part of polyethylene glycol (molecular weight 400) and 1.2 parts of 0.2% color solution are dissolved in approx. 70 parts water at a temperature of approx. 70 ° C. To this solution is slowly added 17.6 parts of ditallow dimethylammonium chloride (75% active and containing about% isopropanol and the remainder water) in molten form, to which 2 parts of Ethomeen T 25 (tallow amine -40% C16 and 60% C18) have previously been added. condensed with 15 moles of ethylene oxide) and 0.62 parts of stearic acid (temperature = 55 ° C) with stirring. A stable product with a viscosity of approx. 100 cps.

Example IX Example VIII is repeated, using the same proportions of cationic material, amine and electrolyte as in Example II and at the same time changing the amount of stearic acid so that the amount is equal to the stoichiometric amount of amine.

Example X Example IX is repeated, replacing the stearic acid with stoichiometric amounts of the following acids: lauric acid, cis-9-dodecenoic acid, myristic acid, cis-9-tetradecenic acid, pentadecanoic acid, cis-9-pentadecenic acid, palmitic acid, cis-9 hexadecenoic acid, heptadecanoic acid, cis-9-heptadecenoic acid, oleic acid, linoleic acid, linolenic acid, elostearic acid, 4-oxo-cis-9-hans-11- -trans-13-octadecatrienoic acid, ricinoleic acid, dihydroxystearic acid, nonadecanoic acid, eicos -11-eicosenoic acid, cis- -9-eicosenic acid, eicosadienic acid, eicosatrienoic acid, arachidonic acid, eicosapentaenoic acid, docosanoic acid, cis-13-docosenoic acid, H 464 139 docosadienic acid, docosatetraenoic acid, 4,8,12,15,19-docosapenta , docosahexaenoic acid, tetracosanoic acid, tetracosenic acid, 4,8,12,15,18,21-tetracosahexaenoic acid and mixtures thereof.

Example XI Examples IX and X are repeated separately, replacing the quaternary substances with those of Example III and repeating all these examples using 1 part of polyethylene glycol (molecular weight 400) in the composition.

The aqueous emollient compositions of this invention are generally useful in the same manner as other such compositions and are particularly suitable in the rinsing step of an automatic washing machine. In these work steps and in any other desired method of treating garments, the compositions are usually used to give active levels of from about 0.005% to 0.3% based on the weight of the clothes, preferably 0.007% to approx. 0.2%. and main from 0a.0.01% u_til ca.0 ', 15%.

Claims (18)

5 10 15 20 25 30 # 64 139 P a t e n t k r a v Stable aqueous concentrated fabric softening composition, characterized in that it comprises (A) 12 to 20% by weight of cationic plasticizer of the formula R1 / R2 + R2 'ia wherein R1, R2, R3 and R4 are aliphatic glycons having 1 to 30 carbon atoms wherein at least one group is alkyl of 14 to 30 carbon atoms; (B) 1 to 5% by weight of an amine salt of an ethoxylated alkylamine and at least one of C 12 - C 18 alkylarylsulfonic acid, C 12 - alkylsulfonic acid, C 12 - C 30 olefin sulfonic acid or C higher fatty acid, preferably C 12 - C 30 fatty acid; and (C) 0.5 - 5% by weight of a water-soluble viscosity regulating electrolyte selected from water-soluble salts of the cations sodium, potassium, lithium, calcium, magnesium and ammonium, preferably sodium chloride, sodium formate, sodium nitrite, sodium acetate. and calcium chloride. Composition according to Claim 1, characterized in that the plasticizer (A) is distearyl dimethylammonium chloride. Composition according to Claim 1 or 2, characterized in that the amine salt (B) is tallow amine with 40% C16 and 60% C condensed with 15 moles of ethylene oxide. 18 Composition according to any one of the preceding claims, characterized in that the ratio between the plasticizer (A) and the amine salt (B) is 40: 1 - 2: 1. 10 15 20 25 30 ig 464 139 Composition according to any one of the preceding claims, characterized in that the plasticizer (A) is present in an amount of about 12% and that the amine salt (B) is present in an amount of about 2%. Composition according to one of Claims 1 to 4, characterized in that the concentration of the plasticizer (A) is 12 to 15% by weight. Composition according to Claim 1, characterized in that in (A) at least one of the groups R 1, R 2, R 3 and R 4 is alkyl having 14 to 30 carbon atoms, preferably 14 to 18 carbon atoms, and the others are lower alkyl, most preferably at least two have 14 to 18 carbon atoms and the others are lower alkyl of 1 to 4 carbon atoms, especially methyl or ethyl, and X is a water solubilizing anion, especially chloride, bromide, iodide, fluoride, sulfate, methosulfate, nitrite, nitrate , phosphate or carboxylate. 8. A composition according to claim 7, characterized in that in (B) the ethoxylated alkylamine is a mixed alkylamine having 10 to 18 carbon atoms fused with from about 5 to about 50 moles of ethylene oxide. Composition according to any one of claims 7, 8, characterized in that in (B) the ethoxylated alkylamine is a C 12 - C 20 amine reacted with from 1 to about 100 moles of ethylene oxide. Composition according to any one of Claims 7 to 9, characterized in that the plasticizer (A) is at least one of distearyldimethylammonium chloride, ditallow dimethylammonium chloride, dihexadecyldimethylammonium chloride, distearyldimethylammonium dimethylammonium bromide, 4; distearyl di (isopropyl) ammonium chloride, distearyl dimethylammonium methosulfate and distearyl diethylammonium chloride. Composition according to any one of Claims 7 to 10, characterized in that in (B) the higher fatty acid is selected from stearic acid, lauric acid, cis-9-dodecenoic acid, myristic acid, cis-9-tetradecenoic acid, pentadecanoic acid, cis-9-pentadecenoic acid, palmitic acid, cis-9-hexadecenoic acid, heptadecanoic acid, cis-9-heptadecenoic acid, oleic acid, linoleic acid, linolenic acid, eleostearic acid, 4-oxo-cis-9-trans-11, trans-13-octadecatriene acid, ricinoleic acid, dihydroxystearic acid, nonadecanoic acid, eicosanoic acid, cis-11-eicosenoic acid, cis-9-eicosenoic acid, eicosadienic acid, eicosatrienoic acid, arachidonic acid, eicosapentaenoic acid, docosanic acid, cis-13-docosenic acid, 12, 15, 19-docosapentaenoic acid, 4, 8, 12, 15, 18, 21-tetracosahexaenoic acid and mixtures thereof. docosahexanoic acid, tetracosanoic acid, tetracosenic acid, Composition according to any one of Claims 7 to 11, characterized in that the electrolyte (C) is at least one of sodium chloride, sodium nitrite, sodium nitrate, sodium formate, ammonium bromide, potassium chloride, lithium acetate, calcium chloride, calcium nitrate and magnesium chloride. Composition according to Claim 12, characterized in that the electrolyte (C) comprises at least one of sodium chloride and calcium chloride. Composition according to any one of claims 1 to 13, characterized in that the electrolyte (C) is present in an amount of at least 0.5% by weight. 10 15 20 25 464 139 15 Process for preparing a composition according to claim 1, characterized in that an aqueous solution of the amine salt (B) in hot water at a temperature of up to 80 ° C is first prepared and then the cationic plasticizer (A) in molten form is added to formation of a gel, cools the gel to below 40 ° C and then adds the electrolyte (C) to break the gel. A method according to claim 15, characterized in that the hot water temperature is about 70 ° C, that the gel is cooled to just below 40 ° C after which the gel is broken, and that the mixture is cooled to room temperature with stirring. Process for preparing a composition according to claim 1, characterized in that one first prepares an aqueous solution of the amine salt (B) in hot water with a temperature of up to 8000, adjusting the pH with an alkaline compound to above about 10, add the cationic plasticizer (A) in molten form, readjust the pH to below 7, cool the mixture to around room temperature and then add the electrolyte (C) to adjust the viscosity. Process for preparing a composition according to claim 1, characterized in that an aqueous solution of the amine salt (B) is first prepared and then the electrolyte (C) is added and then the cationic plasticizer (A) is added in molten form and cooled. the mixture to room temperature.