DE4232448A1 - Process for the preparation of powdered or granular detergent mixtures - Google Patents

Abstract

Powdered or granular detergent mixtures with good cold-water dispersibility are obtained by drying and solidifying, in the prior art manner, mixtures containing: a) quaternary di-fatty acid trialkanol amine ester salts of formula (I) in which R<1>CO is an aliphatic acyl residue with 12 to 22 carbon atoms and 0, 1, 2, or 3 double bonds, n is 2 or 3 and X is halogenated hydrocarbon, methosulphate or methophosphate; and b) hydroxy compounds selected from the group consisting of fatty alcohol polyglycol ethers, polyol fatty acid partial esters and carbohydrates. The products are suitable for the production of laundry revivers and softeners and hair care products.

Description

Field of the Invention

The invention relates to a method for producing powder shaped or granular detergent mixtures in which Ge mix from quaternized difatty acid trialkanolamine ester sal zen and hydroxy compounds in a conventional manner brings solid form.

State of the art

For the treatment of textile fibers, yarns or fabrics is a variety of compounds or mixtures beaten, the desired with the textiles treated with it Impart properties or the components of agents for Are textile care. Depending on the type of active ingredients used can the processing properties, the wearing properties properties of textiles as well as their care the. Cationic ten are usually used for this purpose side, which is particularly light on fibers, fabrics, but can also pull up hair.  

There is always a major technical disadvantage of these products but in their insufficient dissolving or dispersing like in cold water, which is not only the application, but also the production of low-water concentrates considerably more difficult.

There has been no shortage of attempts in the past which to face this problem. For example, the American patent US 34 54 494 fatty acid condensate tion products with an addition of dispersing Polyglycol ethers.

The German patent DE 19 22 046 relates to detergents Containing fatty acid condensation products from fatty acid glycate with a dispersing effect ride included; in German patent DE 19 22 047 these fabrics are also used as textile softeners for liquid laundry aftertreatment agent described. This and similar agents can be dispersed in water by you put them in hot water and mostly high shear forces applies, or by making this from the manufacturing melted condensation product dispersed in water. We Therefore, the manufacturer usually takes the necessary effort introduces the dispersion and provides the user with the Dispersions, which increases with storage and transportation Licher amounts of water connected and thus from economic Point of view is not very profitable.

By using the dispersants mentioned, the further the cold water dispersibility of the above cationic surfactants are improved, this advantage  however, often overcompensated by the fact that the mixtures consist of cationic surfactant and dispersant comparatively poor have other application properties.

The object of the invention was therefore to create a new Ver drive to the manufacture of powdered or granular deters to develop gene mixtures with the help of which products with gu ten advanced properties and satisfactory cold water dispersibility can be provided.

Description of the invention

The invention relates to a method for producing powdery or granular detergent mixtures, in which one Containing mixtures

• a) quaternized difatty acid trialkanolamine ester salts of the formula (I), in which R ¹ CO is an aliphatic acyl radical having 12 to 22 carbon atoms and 0, 1, 2 or 3 double bonds, n is 2 or 3 and X is halide, methosulfate or methophosphate and the molar ratio of fatty acid to trialkanolamine is 1.5 : 1 to 2.0: 1, and
• b) hydroxy compounds selected from the group consisting of Fatty alcohols, fatty alcohol polyglycol ethers, polyol fat partial acid esters and carbohydrates are formed, in a known manner in solid form.

Surprisingly, it was found that the cold water dispersibility of quaternized difatty acid trialkanolamine ester salts by adding the hydroxy compounds mentioned can significantly improve, provided that in the manufacture of Esterquats a well-defined usage ratio of fat acid and trialkanolamine is observed. An impairment the application properties of the products the presence of the hydroxy compounds will not be observed tet.

Quaternized difatty acid trialkanolamine ester salts, so-called "Esterquats" are known cationic surfactants that according to the relevant methods of preparative organic Chemistry can be obtained. A process for their manufacture position is, for example, fatty acids with tri ethanolamine in the presence of reducing agents and under Pass through air and then implement the diester to quaternize with dimethyl sulfate or methyl chloride [WO 91/01 295, Henkel]. Since these are technical products, are always quaternized mono- and triesters in the esterquats included as by-products.

As decisive for the desired effect of a verbes The molar application vers Ratio of fatty acid and trialkanolamine in the production  the esterquats proved. Preferably the components in a ratio of 1.5: 1 to 2.0: 1 and especially in ver Ratio 1.6: 1 to 1.9: 1 used. Become esterquats with a lower fatty acid trialkanolamine ratio, at used for example from 1.2: 1, show the mixtures with the hydroxyl compounds have insufficient dispersibility.

Typical examples of the fatty acid components of the ester quats are caproic acid, caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, elaidic acid, petroselinic acid, linoleic acid, linolenic acid, arachic acid, gadoleic acid, behenic acid and erucic acid, for example, and their technical mixtures, such as their mixtures the splitting of vegetable oils or animal fats. Quaternized difatty acid trialkanol amine ester salts of the formula (I) are preferably used in which R ¹ CO is an aliphatic acyl radical having 16 to 18 carbon atoms, n is 2 and X is methosulfate or chloride. Esterquats based on stearic acid, tallow fatty acid or technical grade elaidic acid are particularly preferred.

Hydroxy compounds of the following come as dispersants Type considered:

• a) fatty alcohols of the formula (II), R ² -OH (II) in which R ^{2 represents} an optionally hydroxy-substituted alkyl and / or alkenyl radical having 12 to 22 carbon atoms. Typical examples are lauryl alcohol, myristyl alcohol, cetyl alcohol, stearyl alcohol, isostearyl alcohol, oleyl alcohol, elaidyl alcohol, petroselinyl alcohol, linolyl alcohol, linolenyl alcohol, ricinolyl alcohol, 12-hydroxystearyl alcohol, arachyl alcohol, gadoleyl alcohol and technical grade alcohol, alcoholic alcohol, behenyl alcohol, behenyl alcohol, behenyl alcohol, behenyl alcohol, and behenyl alcohol, behenyl alcohol, for example, behenyl alcohol, behenyl alcohol, behenyl alcohol, behenyl alcohol, behenyl alcohol, and behenyl alcohol, behenyl alcohol, for example technical fatty acid methyl ester fractions or aldehydes from Roelen's oxosynthesis. Technical C _12/18 coconut _fatty alcohol or C _12/18 tallow _fatty alcohol are preferably used.
• b) fatty alcohol polyglycol ethers of the formula (III), in which R ^{3 represents} an optionally hydroxy-substituted alkyl and / or alkenyl radical having 12 to 22 carbon atoms, R ^{4 represents} hydrogen or a methyl group and m represents numbers from 1 to 40. Typical examples are addition products of 1 to 40, preferably 10 to 25, mol of ethylene and / or propylene oxide onto the alcohols mentioned under a). Addition products of an average of 10 to 25 moles of ethylene oxide with fatty alcohols having 16 to 18 carbon atoms are preferably used, which can have a conventional or even narrowed homolog distribution.
• c) partial polyol fatty acid esters; this includes mono- and / or diesters of polyols with fatty acids of the formula (IV), R ⁵ CO-OH (IV) in the R ⁵ CO for an aliphatic acyl radical having 6 to 22 carbon atoms and 0, 1, 2 or 3 Double bonds stands. Typical examples are mono- and / or diesters of caproic acid, caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, palmoleic acid, stearic acid, isostearic acid, oleic acid, elaidic acid, petroselinic acid, linoleic acid, linolenic acid, arachidic acid, gadoleic acid, behenic acid and technical acid and erucas mixtures with polyols which are selected from the group formed by glycerol, diglycerol, triglycerol, trimethylolpropane, pentaerythritol, glucose or sorbitol. Fatty acid monoglycerides based on fatty acids having 12 to 18 carbon atoms are particularly preferred.
• d) carbohydrates; typical examples are glucose and ins special sorbitol.

The quaternized difatty acid trialkanolamine ester salts and the hydroxy compounds can be in a weight ratio of 50:50 up to 90:10. Products with a special good water dispersibility and excellent avivie properties are obtained when one between the Components a weight ratio of 75:25 to 85:15 sets.  

In a preferred embodiment of the invention Improvement of the cold water dispersibility of the ester quats Mixtures of hydroxy compounds used that have a content from 1 to 10, preferably 2 to 5 wt .-% - based on the Mixture of hydroxy compounds - have sorbitol.

The hydroxy compounds are added to the esterquats preferably not after completion of the end product, but at the level of the non-quaternized esters, i.e. H. in the In the course of the manufacturing process after the esterification of the Fatty acids with the trialkanolamines and before Quaternization. This also has the advantage that the Hydroxy compounds additionally during the quaternization Can take on tasks of a solvent.

The detergent mixtures containing the esterquats are described in solid form, for example as a powder, flake or in particular special granules made available. The shape can - optionally in the presence of solid supports, such as for example zeolites or inorganic salts - e.g. B. in an extruder, a high speed mixer or one Roll pelletizers take place. If desired, the Detergent mixtures also for washing and cleaning typical ingredients such. B. Builder or Control agents included.  

Industrial applicability

The powder obtainable by the process according to the invention shaped or granular detergent mixtures stand out due to good cold water dispersibility and excellent finishing properties with regard to the grip of fibers and textiles.

Another object of the invention therefore relates to the Ver Use of detergent mixtures for the production of finishing agents and fabric softeners in which they are used in quantities of 1 to 50, preferably 10 to 30% by weight, based on the composition, can be included.

The following examples are intended to be the subject of the invention explain in more detail without restricting it.

Examples I. Substances used

A) Quaternized difatty acid trialkanolamine salt
A1) Triethanolamine ditallow fatty acid, quaternized with dimethyl sulfate (Dehyquart® AU-36, Pulcra SA, Barcelona / ES)

B) Hydroxy compounds
B1) dodecyl alcohol
B2) dodecyl alcohol / sorbitol (95: 5 parts by weight)
B3) dodecyl alcohol / sorbitol (96: 4 parts by weight)
B4) Cetyl alcohol
B5) cetyl / stearyl alcohol / sorbitol (96: 4 parts by weight)
B6) cetyl / stearyl alcohol / sorbitol (95: 5 parts by weight)
B7) 12-hydroxystearyl alcohol
B8) Cetyl / stearyl alcohol-20 EO (Eumulgin® B2, from Henkel KGaA, Düsseldorf / FRG)
B9) C _12/14 coconut fatty acid monoglyceride (Monomuls® 90L12, CW Grünau, Illertissen / FRG)
B10) stearic acid monoglyceride (Cutina® MD, Henkel KGaA, Düsseldorf / FRG)
B11) stearic acid monoglyceride / sorbitol (96: 4 parts by weight)

II. Application studies

In a first step, mixtures containing the qua terniert Difettsäuretrialkanolaminester salts and the Hy droxy compounds (weight ratio 85:15) in one High-speed mixer processed into granules.

Then 5 wt .-% dispersions of the granules were in Water (16 ° d, 20 ° C) made and at a rate of 500 rpm until a homogeneous distribution was aimed. The dispersions were stored at 20 ° C and their stability visually over a period of 14 days judges.

The composition of the granules, the time to reach them chen of a homogeneous dispersion and details of it Stability can be found in Tab. 1.  

Table 1

Examination of the dispersions

Claims (11)

1. A process for the preparation of powdery or granular detergent mixtures, in which mixtures containing

• a) quaternized difatty acid trialkanolamine ester salts of the formula (I), in which R ¹ CO represents an aliphatic acyl radical having 12 to 22 carbon atoms and 0, 1, 2 or 3 double bonds, n represents 2 or 3 and X represents halide, methosulfate or methophosphate and the molar ratio of fatty acid to trialkanolamine 1, 5: 1 to 2.0: 1, and
• b) Hydroxy compounds, selected from the group formed by fatty alcohols, fatty alcohol polyglycol ethers, polyol fatty acid partial esters and carbohydrates, in a form known per se in solid form.

2. The method according to claim 1, characterized in that quaternized difatty acid trialkanolamine ester salts of the formula (I) are used in which R ¹ CO is an aliphatic acyl radical having 16 to 18 carbon atoms, n is 2 and X is methosulfate or chloride. 3. The method according to claim 1, characterized in that fatty alcohols of the formula (II) are used, R ² -OH (II) in which R ^{2 is} an optionally hydroxyl-substituted alkyl and / or alkenyl radical having 12 to 22 carbon atoms. 4. The method according to claim 1, characterized in that one uses fatty alcohol polyglycol ethers of the formula (III), in which R ^{3 represents} an optionally hydroxy-substituted alkyl and / or alkenyl radical having 12 to 22 carbon atoms, R ^{4 represents} hydrogen or a methyl group and m represents numbers from 1 to 40. 5. The method according to claim 1, characterized in that one uses as polyol fatty acid partial ester mono- and / or di esters of polyols with fatty acids of the formula (IV), R ⁵ CO-OH (IV) in the R ⁵ CO for an aliphatic acyl radical with 6 to 22 carbon atoms and 0, 1, 2 or 3 double bonds. 6. The method according to claim 5, characterized in that polyols selected from the group are used pe, that of glycerin, diglycerin, triglycerin, trime thylolpropane, pentaerythritol, glucose or sorbitol is forming. 7. The method according to claim 1, characterized in that one uses glucose or sorbitol as carbohydrates. 8. The method according to claim 1, characterized in that the quaternized difatty acid trialkanolamine ester Salts and the hydroxy compounds in the weight ratio 50: 50 to 90: 10. 9. The method according to claim 1, characterized in that the hydroxy compounds the esterquats during the Production after the esterification and before the quater nation closes. 10. The method according to claim 1, characterized in that to bring the detergent mixtures into solid form by they are granulated in a manner known per se submits.   11. Use of powdered or granular detergent Mixtures according to claim 1 for the production of finishing agents and fabric softeners.