FI57609C - DETERGENT COMPOSITION FOR TV TETTING AV TYG - Google Patents

Description

fT-h 'rBi ANNOUNCEMENT Γ π / λ ft [β3 (11) UTLÄGGNINGSSKRIFT 5 760 9 c (45) Taι ·:'. · .ui "-y -: '·'"; · ^ V— ^ (51) Kv.lk?/lnt.ci.3 C 11 D 1/28 ENGLISH —FI N LAN D (21) P »t * nttlh« k «nu * —Pat« «t» n * ölinlng 2516/71 (22 ) H «k # mlip» lv * - Ara6kningtd «g θ8.09 · Τ1 ^ ^ (23) AlkupUvI — GlItighMsdtg 08.09.71 (41) Interpreters for Public - Bllvlt offentllg 10.03-72

National Board of Patents and Registration / 44) NlhUvikslpsnon js kuLLulkalsun pvm. -

Patent · och registerstyrelsen Ansttksn utlagd och utUkriften publicurad 30.05.80 (32) (33) (31) Privilege claimed — Begird prlorltet Q9.09.70 30.03.7i, 16.12.70 England and England (GB) 1 * 3213/70, 8133 / 71, 597 ^ + 1 + / 70 (71) Unilever NV, Burgemeester s * Jacobplein 1, Rotterdam, The Netherlands—

Holiand (NL) (72) James Francis Davies, Wirral, Cheshire, Charles Rowland Gauterin,

Farndon, Cheshire, Philip Alan Gilbert, Wirral, Cheshire, Christopher Charles Storeb, Wirral, Cheshire, England-England (GB),

The present invention relates to solid and liquid detergent compositions. for washing in the washing machine.

Detergent combinations contain an active ingredient and a builder along with other organic and inorganic substances that have specific functions in the wash liquor. The construction material makes it possible for the detergent to effectively use its cleaning effect. Phosphate, for example sodium tripolyphosphate, has often been used as the building material. Recently, however, there has been a concern that phosphates contribute to the eutrophication of lakes and water bodies.

The present invention relates to combinations of substances which contain little or no phosphate, which have good detergent properties and which make textiles soft when washed. These combinations of substances are of the high-foaming, low-foaming or medium-high-foaming type and utilize known compounds of anionic substances, for example alkaryl sulfonate, non-ionic substances and soap (alkali metal salts of long-chain fatty acids).

The detergent combination according to the invention is characterized in that the detergent combination contains 8-25% by weight of? C 10 -C 20 alcohol ethoxylated with 5 to 30 moles of ethylene oxide, a mixture of an unsaponifiable anionic detergent selected from an alkyl aryl sulfonate, an alcohol sulfate, an olefin sulfonate, or a mixture thereof, and alkali metal salts of long chain fatty acids, and 20 to 50 weight percent. a builder consisting of a water-soluble salt or salts of an alpha-sulfonated saturated fatty acid or acids, said fatty acids containing IU-20 carbon atoms, alone or in a mixture with other detergent ingredients, wherein the salt or salts of the alpha-sulfonated fatty acid form at least 10% by weight ? combination of substances, as well as 25 ~ 72 weight? other conventional compatible components of detergent combinations.

The invention relates in particular to low-foam or medium-high-foam detergent combinations containing from 8 to 25% by weight. a mixture of nonionic detergents, anionic detergents and alkali metal salts of long chain fatty acids and 20-50% by weight? a builder consisting of one or more water-soluble salts of alpha-sulfonated saturated fatty acids or mixtures thereof containing salts having 20 to 20 carbon atoms, alone or in admixture with other detergent builder, and 25 to 72% by weight? other known components of detergent combinations. The sulfonated fatty acid salt is used alone or in admixture with one or more known detergent builders, for example so-called dopants which form insoluble calcium salts, for example sodium orthophosphate, sodium alkyl and alkenyl zincinate and malonates, or inorganic compounds, for example sodium hydrofurant tetracarboxylate, sodium pyrophosphate, sodium nitrilotriacetate, sodium methylenediaminetetraacetate, sodium citrate, sodium tartrate, sodium maleate, sodium maleate, trisodium carboxyethyloxysuccinate, Sulfonated both sodium and potassium salts of fatty acids can be used, but as shown below, the sodium salt is recommended. Ammonium salts and, for example, alkyl-substituted ammonium salts and, for example, 57609 amine salts, for example triethanolamine (suitably in liquid combinations) can be used. The combinations of substances may include other known components of alkaline detergent combinations (e.g. silicates), sulphates, germicides, active oxygen carriers, anti-redeposition agents, enzymes, fluorinating agents, perfumes and water.

The combinations of substances mainly contain active oxygen carriers, for example alkali metal perborates, percarbonates or persulphates. Another preferred ingredient is a water-soluble silicate agent, for example sodium silicate. An amount of water is added which is sufficient to give good handling to the powder. And the combination may contain a neutral salt, for example sodium sulphate, may also contain small amounts of substances such as perfumes, anti-redeposition agents, enzymes, germicides and fluorinating agents.

The concentration range given and the types of components are loose because combinations of substances with a known composition can be used in certain varying product concentrations depending on the country in which the combination is to be used. In the USA, detergent powder is usually prepared in a concentration of 0.075-0.5% (w / v) in the product intended for use, while in a product used in Europe, the concentration of the product in use is more usually 0.3-1% (w / v). In the US market, the higher part of the range appropriately given for the salinity of the sulfonated fatty acid, i.e. 35-75% t and for the European market mainly the lower part, i.e. 10-50%. For the US market, the surfactant content of the Powder is mainly 10-50% and the Powder, which is intended for the European market is usually 5-25% · The use of a lower product concentration in the US requires a higher surfactant content in the combination. substance And structural substance.

The thematic active compound combination according to the invention is intended for use in such a way that the concentration of the substance combination in connection with the washing is 0.3 to 0.6% by weight, although other concentrations may also be used.

Between 8 and 25% by weight (mainly 15 to 25% by weight), as given above for a thematic mixture of detergent ingredients, the concentration of detergent ingredients, mainly non-ionically active, is 1-10%. anionic active 4-12% soap 3-8%

The solid combinations according to the invention can be used, for example, in the form of flakes, tablets, powders (for example blown or spray-dried granules and extrudates).

The present invention encompasses the use of synthetic fatty acids as well as natural fatty acids in sulfonated materials. The recommended content of sulfonated, fully cured fatty acid salt is 10-40%. However, according to the invention, it has been found that the alkyl group must consist of at least C 1-4 and mainly C 1-4 in order to obtain a good structural effect. However, this does not mean that a certain amount of C ^ 2 or lower could not be tolerated, but these substances contribute little or no structural effect. Because natural fatty acids are mixtures of fatty acids with different chain lengths, it may be necessary to add a certain amount of these non-effective building blocks to the combination or to perform the separation of the desired chain lengths. The chain length of the sulfonated fatty acid salt is kept as low as possible because increasing the chain length increases the molecular weight and thus decreases the part of the molecule that is available for the structural effect. In addition, the solubility of the salts decreases with increasing molecular weight and it is assumed that sodium salts are irrelevant when the chain lengths are C2q * According to the invention, the C-6 chain has been shown to have optimal structural properties and tallow fatty acid is practically the best source of fatty acid for sulfonation. The potassium salt is more soluble. The use of a potassium salt may require that the other alkali metal salts of the combination be in the predominantly potassium form. 5,57,609 ammonium can also be used and the triethanolamine salt is a particularly useful liquid form in compound combinations.

It is believed that rt-sulfonated fatty acid salts are effective as building materials because they cause the precipitation of alkaline earth metals. It has been found that the combinations of substances according to the invention soften fabrics or textiles when washed and this effect depends on the probable deposition of this precipitate on the surface of the textile material.

It is known that <A-sulfonated fatty acid salts have detergent-active properties, but the invention is based on the use of the properties of these substances as building materials. It has also been shown that these substances soften textiles when washed.

The following are examples of the combinations of substances according to the invention. The combinations of substances were prepared using the ratios given in the following table (by weight). All combinations were of the low / medium foam type, but it was found that the amount of foam obtained increased with increasing amount of sulfonated fatty acid present. The soap chain length distribution was C ^ -2%; C 18-31% t CQ (saturated) -65% and C 1 -C (unsaturated) -2%. These soaps consisted of alkali metals of long chain fatty acids. Sulfonated acids were prepared by the reaction between acid and sulfur trioxide.

Table

Example

Ingredient 12345678 9X 10

Sodium tallow fatty acid alpha sulphonate (fully cured) 20 25 30 35 40 45 34 32 31 29

Sodium soap of hardened tallow fatty acid 45678913 46

Or fatty alcohol 25E0 (fully hardened) 44433266 66 N at riumdecylbenzenesulfonate (055) 88888897 64

Sodium perporate 20 20 20 20 20 20 20 20 20 20

Sodium silicate 88888888 88

The remainder of the combination consisted of fluorescent agents, sodium carboxymethylcellulose, sodium sulfate and water.

57609 6

Analogous potassium-containing combinations were also prepared.

The combinations of substances were compared in terms of washing activity with a typical combination of substances of the standard type, which contained a phosphate structuring agent and having the following composition.

Sodium dodecylbenzenesulphonate (055) 9%

Non-ionic (fully cured) tallow fatty acid alcohol 25E0 2.5%

Sodium tripolyphosphate 55%

Sodium perporate 20%

Sodium silicate 5%

The remainder consisted of sodium sulfate, water, sodium kerboxymethylcellulose, and a fluorinating agent.

The standard detergent combination proved to have a washing capacity of 59.0 at 50 ° and 70.1 at 70 °. Washability was added using a dacron / cotton test cloth, soiled with artificial sebum and dust mousse in water, having a hardness of 18 ° H (calcium: magnesium ratio oil 2: 1). The agent of Example 1 was found to have a washability of 54.8 at 50 ° and 69.9 at 70 °, the agent of Example 6 had a washability of 61.7 and 74.9 at these temperatures, respectively. The detergency of these combinations of substances according to the invention was thus comparable to that of the standard combination of substances. The substances of Examples 2, 3, 4 and 5 had a washing capacity of the order of magnitude that was between the values of Example 1 and Example 6.

The percentage washing capacity (D) was determined with an "Elrepho reflectometer" type apparatus for measuring the following parameters:

Rc - reflectivity of the detergent Rs - reflectivity of the soil Rw - reflectivity of the detergent

In which case the following formula was used in the calculation

The contaminated material was washed in 0.6% solution solution for 10 minutes in a "tergotometer" nitrogen apparatus using 7 57609 90 oscillations per minute and for 2 minutes in water having a hardness of 18 ° H (French).

The combinations of substances according to Examples 7, 8, 9 and 10 make it possible to study the effect of the variation in the amounts of the components of the granular mixture. I obtained the detergency values given in the following table:

Table

Eg 50 ° C to 70 ° C

7 63.0 70.4 8 61.3 70.4 9 57.7 70.8 9 (potassium analogue) 58.6 70.6 10 55.7 69.9

The potassium analog of Example 9 was prepared using potassium salts instead of sodium salts in all alkali metal components in the substance combination. These combinations of detergents had a satisfactory washability compared to a standard combination of detergents with a washability of 58.3 and 64.2 at 50 ° and 70 ° under the same experimental conditions, respectively.

It is expedient for the combination of substances according to the invention to be used at a pH of more than 9.5 in the washing liquid.

The present invention thus relates to low and medium high foam phosphate-free detergent combinations with good washing properties. Replacement of the phosphate builder component with a sulfonated fatty acid salt has been accomplished without adversely affecting the foaming tendency, which is desired to remain low. The combination of substances according to the invention can be made in powder form with good results.

Example 11 <Sodium salt of X-sulfocured tallow fatty acid 17.5%

Sodium orthophosphate 7.5%

Alkylbenzenesulfonate 10.0%

Sodium salt of long chain fatty acids 4.5%

Tallow fatty alcohol 25E0 2.0%

Alkaline sodium silicate 8.0%

Palm palm ethanolamide 22.0% S 57609

The remainder is sodium carboxymethylcellulose, sodium sulfate, stabilizers.

This combination of substances, which demonstrates the utility of the sulfonated fatty acid with the phosphate builder, proved to have a detergency substantially equivalent to that of the compound containing sodium tripolyphosphate as a builder.

All the combinations of substances given in the examples proved to have an emollient effect on textiles compared to the combination of substances containing sodium tripolyphosphate as a building material.

Example 12

An experiment was performed to demonstrate acceptable washing properties in combinations of substances containing salts of <A-sulfonated fatty acids as a builder. Products were evaluated using a "tergotometer" type apparatus on a test cloth (dacron / cotton) soiled with dust-sugar dust and in a washing machine with a naturally soiled object.

Combinations constructed with sulfonated fatty acid salts have been shown to be comparable to an agent containing alkyl benzene sulfonate / sodium tripolyphosphate at concentrations of both 0.1% and 0.15% w / v. The experiments were performed using the following combinations of substances: sulfur sulfonated fatty acid salt 15-65%

Alkylbenzenesulfonate 18%

Alkali silicate 10%

Sodium sulphate about 12%

The experiments were performed using a washing liquid with a hardness of 18 ° (calcium: magnesium ratio 2: 1) at 50 ° or 60 ° and village rinse aid in the same water with a hardness of 18 ° H (French definition of hardness, i.e. 1 ° H = 0 , 0001 M calcium). Apart from alkylbenzene sulfonate, detergent olefin sulfonates, sulfonate type "Dobanol 45 5E0" and "Tergitol 15-S-7" proved to be comparable to the alkyl benzene sulfonate / sodium tripolyphosphate combination. Table I gives the results measured with a "tergotometer" type device, in which the reflectance is given as a percentage.

9 57609

Table I

Pesukvkv

Higher values mean better washing ability.

Ingredient content 15% 25% 35% 45% 55% 65% (a) washing liquid temperature 50 ° C, product concentration in the washing liquid 0.15% w / v

Sodium fatty acid sulphonate 40 60 62 64 65 66

Sodium tripolyphosphate 50 59 62 60 bl 62 (b) washing liquid temperature 60 ° C, product concentration in the washing liquid 0.6% w / v

Sodium fatty acid sulphonate 61 67 67 68 *

Sodium tripolyphosphate 61 68 68 69 * ^ product concentration 0.3% w / v

Blown powders were also tested both without and with the enzyme containing alkylbenzenesulfonate (Oronite 1060) as a surfactant, and these blown powders proved to be satisfactory.

To demonstrate the softening effect of textiles and fabrics, a combination of a substance containing a salt of a β-sulfonated fatty acid (50%) and an alkylbenzenesulfonate (16%) was studied. A scavenger combination containing 20% alkyl benzene sulfonate was also studied. After washing according to the above procedure for testing the washing ability, the fabric was dried in a tumble dryer and the fabric was sampled after certain washes and the softness of the sample was compared with similarly prepared samples washed using standard combinations A, B and C given below.

Standard A B C

Dodecylbenzenesulphonate 18 9 12

Tallow fatty alcohol sulfonate 0 9 0

Soap 0 0 4

Sodium tripolyphosphate 40 50 47

Alkali silicate 6 67

Sodium carbonate 0 20

Sodium sulphate 30 20 20 dissolves part of water and perfume 10 57609

Table II gives the number of washes for each fabric and the number of persons on the test panel who considered it the softest of the fabric, which had been washed with a combination of substances containing r * -sulfonated and fatty acid as a building material. The combination containing 16% alkylbenzenesulfonate was tested at a product concentration of 0.15% and the combination containing 20% detergent ingredients at a product concentration of 0.075, 0.1 and 0.15%. · These experiments show the better fabric softening properties of the combinations according to the invention.

Re-precipitation was also studied using different grades of textiles and fabrics also with the standard material combinations B and C given above. Recrystallization was measured as loss of reflectivity after 25 wash cycles (see Table III) using a product concentration of 0.15%. The product (D) of the invention contained 50% sodium fatty acid sulfonate and 20% alkylbenzenesulfonate as detergent active ingredients.

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Table III

Re-precipitation

Loss of resilience after 25 washes.

Subject B CD

Cotton sheet 1.6 1.7 0.7

Dacron / cotton (thick)

Dacron / cotton (thin) 2.3 10.3 0.9

Krimplene 20.9 40.1 2.9

Terry hand towels 4.4 3.9 4.2

Nylon 13.1 15.5 8.3 The present invention thus relates to detergent compositions containing <* r sulfonated fatty acid salts as a building material. These combinations of substances have properties comparable to those of combinations of substances which contain sodium tripolyphosphate as a building material. Sulfonated fatty acids generally have an iodine value greater than 1. The use of a more unsaturated substance gives a colored product which requires further purification / bleaching before use.

Table III re-deposition of 25 washes with reflection loss

Subject B CD

Cotton sheet fabric 1.6 1.7 0.7

Dacron cotton (thick) 1.6 15.6 0.1

Dacron cotton (thin) 2.3 10.3 0.9

Krimplene 20.9 40.1 2.9

Terry Towel 4.4 3.9 4.2

Nylon 13.1 15.5 8.3

Example 13

A series of detergent powders were prepared containing:

Linear alkyl (C 1-4) benzenesulfonate 0-70%

Sodium sulphonated saturated fatty acid (C18 65% + Cl6 35%) 70-0%

Alkaline silicate 10%

Sodium sulphate, water, soap 20% 13 57609 The total amount of active + sulphonated fatty acid salt was always 70%.

Washing capabilities were determined using a Terg-O-Tometer at 90 rpm. The product concentration of the washing liquid was made 0.15% in 18 ° hard water (calcium: magnesium = 2: 1). Washing at 50 ° C for 10 minutes was followed by a one minute rinse at 35 ° C. The test garment was dacron / cotton with dirt dust.

The amount of soap (alkali metal salts of long chain fatty acids) was about 1/9 of the amount of sulfonated fatty acid salt.

Washing performance, measured as a percentage, is shown in the continuous curve 1 in Figure 1. It is seen that the recommended ranges are: active detergent 10-60% sulfonated fatty acid salt 6-10%

The most preferred ranges are 20-50% for the active ingredient and 50-20% for the sulfonated fatty acid salt. It is to be understood that in commercial formulations, the total amount of active substance + structural agent does not normally correspond to 70% of the total amount.

The ranges performed for the ratio of active ingredient to structural agent are 1: 6-6: 1 and the most preferred is 2: 5-5 * 2.

Curve 1 in the figure shows the increase in washability achieved by adding sulfonated fatty acid salts to a linear alkyl benzene sulfonate.

Example 14

Example 15 was repeated using secondary Calcol 9 EO (Tergitol 15-S-9) (nonionic) as the active ingredient. The product concentration was 0.1%.

The dotted curve II in the figure shows the washing capabilities achieved. Expressing the recommended ranges as a percentage of the total, we obtain icnito active ingredient 5-30% sulfonated fatty acid salt 40-65% 44 D 7 w ϋ 'j

The most preferred ranges are 10-20 ϊό for the nonionic active ingredient and 50-60% for the sulfonated fatty acid salt. It will be appreciated that in a commercial formulation, the total amount of active ingredient in the active ingredient will probably not correspond to 70% of the total combination of substances. Recommended ranges for the ratio of active ingredient to structural agent are 1: 13-5: 4, most preferred 1: 6-2: 5. Curve II shows the increase in washing capacity obtained by adding the salt of the β-sulfonated fatty acid to the nonionic active substance.

Example 15

Example 13 was repeated using a secondary alkali sulfonate (C 1 -C 17 chain length) as the active ingredient. The product concentration was 0.1%, Dot / Dashed Line 3 in the figure shows the washing performance achieved. Expressing the recommended ranges as a percentage of the total, we obtain the active time sulfonate 5-50% sulfonated fatty acid salt %

The most preferred ranges are 10-35% for the active alkane sulfonate and 35-60% for the sulfonated fatty acid salt. Expressed as the ratio of active substance to structural agent, the preferred ranges are 1: 13-5: 2, with the most preferred ratios being 1: 6-1: 1. It should be noted that the addition of a salt of a s <-sulfonated fatty acid increases the detergency of the active ingredient.

The active alkane sulfonate can be prepared by reacting a sulfonyl chloride (SO 2 Cl 2) with a straight chain alkane using ultraviolet light. The position of the sulfone group is arbitrary along the chain. The active substance used in this example was obtained from the German company Hoechst AG.

Example 16 This example illustrates the criticality of the chain length of a sulfonated fatty acid salt.

A series of formulations were tested containing:

Linear alkyl (C 1-4) benzene sulfonate 20 μl

Sodium structural salt 50%

Alkaline silicate 5 gen

Sodium sulphate, water 25 / -is is 57609

In the Terg-O-Tometer and the washing capacity was measured as a percentage. The test garment was dacron / cotton soiled with vacuum cleaner dust.

A 0.1% product concentration was used in 18 ° hard water (calcium: magnesium = 2: 1), and the pH was initially adjusted to 9.5. The disodium salts of the α-sulfonated fatty acids listed below were compared with sodium tripolyphosphate (STPP) as a building block.

Fatty acid Washing capacity (%)

Stearic acid (Cl 2) 44.7

Palmitic acid (C- ^ g) 37.2

Hardened vegetable oil (C ^ g 65%: C ^ g 35%) 38.1

Palm oil (C ^ g 50%: C ^ g 50%) 36.3 C13 n'3 STPP 38.3

Claims (7)

1. Detergent composition for washing fabric, characterized in that the composition contains 8 to 25% by weight of a mixture of a C 1 -C 20 alcohol ethoxylated with 5 to 30 moles of ethylene oxide, a non-free anionic detergent active substance which is alkylarylsulfonate, alcohol sulfate, olefin sulfonate or their mixture, and alkali metal salts of long-chain fatty acids, and 20-50 wt. 20 carbon atoms, alone or in admixture with other detergent builders, wherein the alpha-sulfonated fatty acid site or salts comprise at least 10% by weight of the blank composition, and 25-72% by weight of other usual suitable components for the detergent composition. Composition according to claim 1, characterized in that the alpha-sulfonated fatty acid contains from 16 to 20 carbonate omers. 3. Detergent composition according to claim 1 or 2, characterized in that it contains 10-40% by weight of salts or salts of alpha-sulfonated fatty acid. 4. Detergent composition according to any one of claims 1, 2 or 3, characterized in that the salt of the alpha-sulfonated fatty acid is sodium salt. 5. Detergent composition according to any preceding claim, characterized in that the present alpha-sulfonated fatty acid contains at least 50% by weight of C 6. Detergent composition according to any of the preceding claims, characterized in that the detergent active substances are included in the following contents: nonionic active material 1-10% by weight anionic active material 4-12% by weight of long chain fatty acids 3-8% by weight 7. Detergent composition according to any of claims 1-6, characterized in that the amount of the mixture of the detergent active substances present is 15-20% by weight.