FI57271C - FRAMSTAELLNING AV TVAETTMEDELSFORMULATIONER - Google Patents

Description

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England-England (GB) 1 + 7193/7 ^

Proven-Styrkt (71) Unilever N.V., Burgemeester s'Jacobplein 1, Rotterdam, The Netherlands (NL) (72) Richard Shav Johnson, Wirral, Merseyside, John Kenneth Potter,

Wirral, Merseyside, England-England (GB) (7 * 0 Leitzihger Oy (5 ^) Preparation of Detergent Formulations - Framställning av tvatt-Medels formulati oner The present invention relates to the granulation of detergent formulations.

A solid detergent formulation is usually prepared for marketing as a granular mass. Commercially used manufacturing methods for these granules include spray drying, spray cooling, and dry blending. These methods are used to form granules having a diameter of about 0.3 to about 3 mm. These methods can be used in combination, for example, the ingredient can be dry blended into a spray-dried product.

Pending patent application gb 48420/72 (corresponding to German patent application 2,352,393) describes the use of a device with a base table rotating inside a cylindrical smooth side wall for granulating a detergent formulation made of powdered components. In this previously described method, detergent components in powder form are formed into a substantially horizontal annular rotating layer and contacted with a liquid binder that can be released from the component during rotation. This device is described in U.S. Patent 3,277,520.

In the present invention, this device is used by a granulation technique based on another non-extrusion of granules formed.

2 57271 for post-granulation treatment. The detergent formulation is thus first prepared in granular form, for example by spray-drying the slurry of the mixture or by aggregating the powder components, for example by pan granulation, and then treated with the apparatus described previously. Another device that can be used for the initial granulation step consists of an open bowl with a vertical axis in the middle. The cup is mounted on a vibrating table, which gives the cup a gyrostatically oscillating motion. There is a rolling and collapsing motion in the matter in the cup. An example of such a device is the "Vibro-Energy" coating machine marketed by William Boulton of Burslem, England. The post-granulation device shown here is known as an extruder balling device. The handling of extruded materials is not included in this application.

Using this post-granulation treatment, the bulk density of the formulation can be selected to suit the formulation. When formulating detergents, it often happens that a component of the formulation is changed and, under the conditions previously used in the treatment, a formulation with a different, lower bulk density can be obtained. If an earlier high pulp density is to be obtained, considerable work must be done to change the processing parameters in order to obtain the previously achieved density. It should be noted that there is a limit to the increase in mass density that can be achieved by the method of this invention; usually the growth is not more than 60% of the initial mass density. The post-granulation treatment is performed without the addition of a binder.

The sealing treatment preferably takes at least about 1/2 minute, preferably 3 minutes. Compaction is best continued until the density of the 3 masses has increased by at least about 0.1 g / cm.

By using the described device, a uniform mass density can be achieved even when there are changes in the components of the formulation in the first granulation step. The treatment performed in the proposed device increases the bulk density; the increase depends on the processing time. Thus, by changing this parameter in a subsequent processing step, formulations with similar bulk densities can be obtained. Mass densities between 0.25 and 1 g / cm can be obtained by the process of this invention. The time that can be allowed to elapse between the granulation step and the post-granulation step depends on the granulation method used. In some granulation processes, the increase in bulk density achieved by a normal post-granulation treatment decreases with increasing time between steps.

The device used in the post-granulation process according to the invention consists of a substantially vertically arranged smooth side wall, for example a cylinder, in the middle of which a rotating roughened, preferably horizontal table is placed concentrically. This table can rotate about the central axis of the side walls so that there is relative movement between the table and the side walls.

The degree of roughening of the table is selected depending on the method in question and the table is placed slightly apart from the side walls and the roughening may come from the manufacture. One manufacturer of this type is manufactured by Fuji Paudal KK (formerly Fuji Denki Kogyo KK), Japan, under the trade name "Marumerizer". This device is described in German Patent 1,294,351 and U.S. Patent 3,277,520 (reissued under number 27214) and in Japanese Patent 8684/1967.

The detergent formulation used in the present invention contains a detergent active agent. This active substance or mixture of active substances is selected from the group consisting of known anionic, cationic, nonionic, amphoteric and zwitterionic active substances. Examples of commercially known active ingredients are alkaryl sulfonates, for example dodecylbenzenesulfonate, C 1 -C 20 alkyl sulphates, sulphonated olefins (C or straight-chain salts of long-chain fatty acids (C1-C2-C2q). The salts are usually sodium salts, but potassium ammonium and other water-soluble salts are also useful. Examples of active substances are given in Schwartz, Perry and Berch, "Surface Active Agents and Detergents, Volume II (1958).

Detergent builders may also be present, for example precipitating builders which form insoluble calcium salts, for example sodium orthophosphate, carbonates and sodium alkyl and alkenyl succinates, sulphonated fatty acid salts, and malonates, for example. sodium pyrophosphate, sodium nitrilotriacetate, sodium ethylenediamine-4,5271 tetraacetate, sodium citrate, sodium tartrate, sodium malate, trisodium carboxymethyloxysuccinate, sodium oxide acetate and sodium acrylate, sodium hydroxide succinate, and also polyelectrolyte such as

Temporary salts, for example sodium silicate, may also be present.

Bleaching agents may be present, for example active oxygen scavengers, for example perborates, percarbonates; best these are about 5 to about 30%. Other additives that are usually present in relatively small amounts include anti-redeposition agents, perfumes, fluorescent agents, germicides.

The detergent formulation usually contains from about 5% to about 30% by weight of detergent active agent and detergent builder in the same range. The amount of active substance may be outside these limits in special formulations, i. about 2 to about 40 weight percent.

The amount of detergent filler may also be outside this recommended range, i. about 5 to about 60 weight percent; the bulking agent is used in larger amounts in formulations intended to be used in relatively low concentrations, for example in the washing of fabrics.

The product produced by this method looks similar to the products obtained by known methods, for example spray-drying, and is therefore accepted by the consumer in a commercial product. In the following, the invention is illustrated by way of examples without limiting it.

Example 1

In the granulation step, a pan granulator with a diameter of 500 mm and a depth of 250 mm was used. It was operated at an angle of 30 ° to the horizontal at a rotation speed of 22 rpm. The formulation given below was mixed as a powder and a 5 kg batch was granulated in a pan by spraying water on as a binder.

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Ingredient Quantity (% by weight)

Sodium dodecylbenzenesulphonate 15.6

Coconut ethanolamide 2.2

Sodium tripolyphosphate 35.6

Alkaline silicate 6.7

Sodium sulphate 18.4

Sodium perborate 21.1

Smaller additives

The bulk density of the product was 0.56 g / cm. Immediately after preparation, 1 kg of product was placed in a Marumerizer with a diameter of 230 mm. The product was post-granulated with this device at a rotation speed of 1160 rpm. After 5 minutes, the bulk density 3 had increased to 0.91 g / cm 3. Examining the product at different times, the density was found to be 0.69 after 0.5 minutes, 0.71 after 1 minute and 0.82 after 3 minutes.

Example 2

Example 1 was repeated with the following formulation.

Ingredient Quantity (% by weight)

Sodium dodecylbenzenesulphonate 8.3

Sodium stearate 4.7

Non-ionic surfactant 2.6

Sodium tripolyphosphate 42.0

Alkaline silicate 6.8

Sodium sulphate 7.4

Sodium perborate 27.3

Minor Additives 0.9 In this formulation, water containing a suitable amount of the above nonionic active agent 3 was used as a binder for granulation. The mass density of the granules was initially 0.56 g / cm and after treatment for 4 minutes in a Marumerizer, the mass density had risen (limit) to 0.87 g / cm.

57271

Example 3 This example illustrates the post-granulation treatment of a spray-dried product. The following formulation was slurried in water to a dry matter content of 55% and spray dried in the normal manner.

Ingredient Quantity (% by weight)

Sodium dodecylbenzenesulphonate 9.1

Sodium stearate 12.5

Non-ionic active substance 6.0

Sodium tripolyphosphate 50.0

Alkaline silicate 6.8

Sodium sulphate 14.8

Smaller additives

The bulk density of the spray-dried product was initially 0.34 g / cm. After 10 minutes, it was post-granulated for 10 minutes in a Marumerizer 3, increasing its bulk density (limit) to 0.52 g / cm 3.

Example 4

The formulation containing the ingredients listed below was granulated in a vibrating dish previously described in the introduction.

Ingredient Quantity (% by weight)

Sodium dodecylbenzenesulphonate 21.5

Sodium tripolyphosphate 34.4

Alkaline silicate 6.5

Sodium sulphate 14.0

Sodium perborate 21.4

Coconut ethanolamide 2.2 4 g of a powdered formulation was fed into the machine and granulated by spraying 600 g of water as a binder over 10 minutes. The granulated product was removed and the excess material (greater than 1 mm) was screened apart.

3

The mass density of the screened product was 0.64 g / cm. 1 kg of product was fed to a Marumerizer (diameter 230 mm) and treated for 5 minutes at 1160 rpm. The time between the removal and the post-granulation step was 5 minutes. The bulk density increased to 0.75 g / cm.

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Example 5 This example was performed to show how the increase in mass density decreases with increasing time between the two steps of the process. Example 1 was repeated by allowing different time intervals to elapse between granulation and post-granulation? the results are given in the following 3 table. The bulk density was 0.64 g / cm immediately after granulation.

Time between steps Mass density (g / cm 2) (minutes) _ after post-granulation 0 0.90 30 0.89 50 0.83 60 0.75 120 0.67 240 0.65

Example 6

The following formulation was granulated in a pan granulator, after which its bulk density was increased.

Dodecylbenzenesulfonic acid 1.48 kg

Sodium tripolyphosphate 3.20 kg

Alkaline sodium silicate powder 0.60 kg

Sodium sulphate 1.50 kg

Sodium perborate 1.90 kg

Sodium carbonate (hammer ground) 0.25 kg

Water 1.00 kg

With the exception of sulfonic acid and water, the components were fed to a pan granulator (diameter 500 mm) at an angle of 30 ° to the horizontal and rotated at 22 rpm. Acid was sprayed on at 60 ° C together with the air used to spray it at a temperature of 100 ° C and a pressure of 1.4 kg / cm 2. At the same time, water was sprayed on. The mixture was worked up until the product was granulated, at which point it was removed and compacted by post-granulation in a Marumerizer (230 mm diameter) which was rotated for 5 minutes at 1160 rpm.

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After removal from the pan granulator, the bulk density was 0.53 g / cm 3 and after compaction 0.78 g / cm 3.

Example 7

Example 6 was repeated with the formulation:

Dodecylbenzenesulfonic acid 0.64 kg

Hardened tallow fatty acids 0.74 kg

Tallow alcohol, ethoxylated with an average of 18 moles of ethylene oxide (non-ionic) 0.40 kg

Sodium tripolyphosphate 3.30 kg

Alkaline sodium silicate 0.42 kg

Sodium sulphate 1.00 kg

Sodium perborate 2.50 kg

Sodium carbonate (hammer ground) 0.25 kg

Water 1.00 kg

The sulfonic acid was atomized in a mixture with a fatty acid and a nonionic active substance using air at a pressure of 1.4 kg / cm and a temperature of 150 ° C. The samples were compacted (1160 rpm, 5 minutes) after times of a certain length. Mass density first increased with time, but then decreased. This shows the effect of the time between successive treatments on the final mass.

3

Mass density after pan granulation 0.51 g / cm immediately after compaction 0.80 g / cm3 interval 0.5 hours 0.82 g / cm3 interval 1 hour 0.86 g / cm3 interval 2 hours 0.83 g / cm3 interval 5 hours 0.85 g / cm 3 * interval 7.5 hours 0.87 g / cm 3 interval 17 hours 0.75 g / cm 3 interval 24 hours 0.74 g / cm 3.

Claims (8)

9 57271 A process for preparing a detergent composition in granular form, characterized in that the mixture is granulated by a non-extrusion process and then treated in a substantially horizontal circular rotating bed in a post-granulation apparatus consisting of a substantially horizontal, roughened substantially rotatable table located substantially vertically at the bottom, so long that the bulk density of the granular mixture increases. A method according to claim 1, characterized in that the time is at least about 1/2 minute. A method according to claim 2, characterized in that the time is at least about 3 minutes. Process according to one of the preceding claims, characterized in that the increase in mass density is at least about 0.1 g / cm 2. Process according to one of the preceding claims, characterized in that the granules are formed into a slurry of a mixture of spray-dried sludge. Process according to one of Claims 1 to 4, characterized in that the granules are formed by agglomerating a mixture of the powder components of the mixture. Process according to any one of the preceding claims, characterized in that the mixture contains from about 2% to about 40% by weight of detergent, preferably from about 5% to about 30%. Process according to one of the preceding claims, characterized in that the mixture contains from about 5% to about 60% by weight, preferably from about 5% to about 30%, of a builder.