NL8203840A - DOSAGE UNITS FOR A DETERGENT, METHOD OF MANUFACTURING AND APPLICATION THEREOF. - Google Patents

Description

VO 3786 ι

Dosage units for a detergent process for manufacturing and use thereof.

The invention relates to a detergent dosage unit comprising surfactants and auxiliaries suitable for this use and to a method of preparing such dosage units and an application.

Many proposals have already been made to prepare dosage units for a detergent, for example, in U.S. Pat. Nos. 4,099,912, 4,23,4,442, 4,219,435 and in Norwegian Publication No. 130,594. However, it has hitherto been not possible to provide detergent dosage units such as tablets in clay sizes which can be used with great efficiency to solve a wide variety of cleaning problems. This is probably due to the fact that it has hitherto not been possible to prepare a surfactant mixture at a reasonable cost, which is satisfactory and effective even when used in small amounts. In addition, it is usually difficult to manufacture tablets that include surfactants and that have sufficient mechanical strength, sufficient storage stability, easy decomposition in water, and high cleaning effect at a small concentration in an aqueous cleaning agent. liquid.

Surprisingly, it has now been found that a highly effective dosage unit of a detergent can be manufactured which contains surfactants and auxiliaries suitable for the intended use by using as previously active components a mixture of per se known per se known surfactants with one or more compatible fluorine-containing surfactants Λ selected from the fluorine-containing anionic, nonionic, cationic and amphoteric surfactants. Such a mixture has a synergistic cleaning effect in that adding only 001% by weight of fluorine-containing surfactants to the detergent mixture of an otherwise known type has a surprisingly great cleaning effect, even when used, in a concentration which is unprecedentedly low for detergent mixtures of this type 8203840 I> 2.

In a dosage unit of a detergent according to the invention, the mixture of surfaces consisting of up to 99.99% of conventional surfactants and from 0.01 to 100% by weight of one or more compatible fluorine-containing surfactants consists of active substances, the latter of which may be anionic, non-ionic, cationic or amphoteric.

In view of the high price of the fluorine-containing surfactants, an amount of these compounds is preferably used as small as possible for the intended use.

The optimal amount can be determined in each case by tests.

As stated, a dosage unit according to the invention may optionally contain adjuvants, which are of course selected to match the other ingredients of the mixture in the dosage unit. Thus, by suitable selection of the auxiliaries, a desired pH value can be achieved in the aqueous solution of the dosage unit. For example, the dosage unit may also contain a color-forming component that matches the pH value (eg, a red color for a pH below 6, a green color for a pH of 6-8, and a blue color for a pH above 9). or disinfectants, pesticides and fragrances.

Examples of suitable conventional surfactants are, for example, those cited in U.S. Patent 4,099,912, and the contents of that disclosure are incorporated herein by reference. A suitable surfactant supplied by BASF is sold under the trademark "Lutensit AN 10".

In this US patent specification a series of commonly used excipients are mentioned. As examples of acids which can be used for the preparation of an acid powder which has been inactivated on its surface for use in the preparation of a preferred embodiment of a dosage unit according to the invention, mention can be made, for example, of the polyvalent carboxylic acids, such as citric acid, lactic acid , gluconic acid, trinitriloacetic acid sulfamic acid and inorganic acids such as boric acid.

As examples of suitable fluorine-containing surfactants, mention may be made in particular of the fluorine-containing surfactants selected from the fluorocarbon-containing surfactants having 4-20 carbon atoms in the fluorine-containing carbon chain which 7 - 2S have fluorine atoms and the compounds of one of the formulas

CnF2n ± lC6H4-X '

CnP2nilS02X '

CnF2n-lC0X '

CnF2n-1X '10 CnF2n-1C2H4X' and C / 2nilC6VS02 ^ where in the case of anionic surfactants the X represents a 12 3 - -OH, -NR R, -NHR ^, -NHCH ^ OOH, -SC> 3 _ -SH, -CSSH, RjPC ^, etc., while in the case of nonionic surfactants X represents -N (R4) CO (OCH-CH2} (OCH-CH) -) OC.HQ 2 2 n 3 2 n 4 9 and - (0CH, -CHJ -OH, -CN, -SON etc., 2 2n and in the case of cationic surfactants X represents 20 -NCH- H. (CLH_) = R + y "*, where Y is a halogen atom and 2 4 2 3 2 in the case of amphoteric surfactants, the X represents + 12 -NCH2H4N (RR) C2H4 = COO etc.

Suitable anionic fluorine-containing surfactants are marketed by 3M under the trademarks "Fluorad-FC 128", "Fluorad-PC 170 C", and "Fluorad-FC 430".

The fluorine-containing surfactants suitable for use according to the invention are either already known mixtures or new mixtures, which can be prepared in a manner known for analogous compounds.

It has hitherto been considered impossible to obtain a useful fabric softener unless it has been prepared in a liquid state in the usual manner. Surprisingly, it has now been found possible to process a conventional softener in a tablet according to the invention, which, after disintegration of the tablet in water, is equally effective as conventional softeners. A particularly advantageous embodiment of the invention is therefore a dosage unit in which a fabric softener or auxiliary material is incorporated.

Active wax-containing car washes have hitherto not been supplied in the form of tablets. It has hitherto been necessary to prepare such mixtures in the form of liquid products in a traditional manner. Surprisingly, however, it has been found possible to prepare an effective car wash detergent in the form of a dosage unit, for example as a tablet, which is a dosage unit of the invention. When such a wax-containing tablet according to the invention is placed in hot water, the tablet easily disintegrates, immediately following an aqueous emulsion of wax which, when used, yields an excellent film or coating of wax, without streaking being formed. the treated surface.

A dosage unit according to the invention is preferably supplied in the form of a tablet or a powder, which is filled, for example, in capsules, bottles, pouches, packages or pads. A preferred tablet size is 5-100 g with a volume of 3-800 ml. The tablets can be cylindrical with a diameter of 5 - 20 mm and a height of 5 - 150 mm, or rectangular, for example with sizes in the range between 5 x 5 x 5 mm and 30 x 30 x 150 mm. For the manufacture of a dosage unit according to the invention it is. usually necessary to use a special technique to avoid problems during manufacture, which may include, for example, attack by moisture from the air, flow or deformation of a hydrated hard and practically insoluble layer on the surface of the tablet.

The method according to the invention for the production of a dosage unit of a detergent containing the surfactants and auxiliaries is characterized in that a mixture is prepared, with the exclusion of moisture, of which 0 - 99.99% by weight is used. surfactants with 0 µl - 100% by weight of one or more compatible fluorine-containing surfactants selected from the anionic, nonionic, cationic and amphoteric surfactants, to distribute this mixture evenly a mixture of the selected adjuvants such that the particles of the adjuvant are coated with a layer of the surfactant mixture and the thus stabilized powder is mixed with an acid powder of which the surface is inactivated, after which the powder obtained is optionally tableted or filled in capsules, bottles, bags, 5 packs or pads.

With the process according to the invention it is surprisingly possible to process a very large amount of liquid active substance without clumping occurring into a water-insoluble mixture.

A special embodiment of the method according to the invention which leads to a dosage unit in the form of a tablet with a long dissolution time, is characterized in that a mixture of 0 - 99.99% by weight of conventional surfactants is prepared with the exclusion of moisture. with 0 j) l - 100 wt.% of one or more fluorine-containing surfactants compatible therewith which may be anionic, nonionic, cationic or amphoteric and distribute this mixture evenly over the mixture of adjuvants containing binders which slowly dissolve in water such that the particles of the adjuvants are coated with a layer of the surfactant mixture, after which the thus stabilized powder is tableted to a preferably elongated tablet.

Dosage units made in accordance with the invention are mechanically strong, but nevertheless, if desired, they may have such a shape that they easily disintegrate in water. For pressing the tablets, a pressure of 30-800 kg / m 2 can be used, resulting in a density of 0.7-2.0 kg / cm 2.

The dosage units according to the invention can be used in many fields, for example for domestic use, in hospitals and laundries, on farms, in the food industry and also in the iron and metal industry. The dosage units of the invention are particularly in the form of tablets suitable for use in the preparation of detergent solutions for high pressure cleaning. Heretofore, it has not been possible to supply a detergent product for high pressure cleaning in the form of a tablet.

The invention is further illustrated by the following 8203840 6 examples, but is not limited by those examples.

Example 1

A detergent mixture for car washing is prepared from the following components: 5 Components parts by weight "Fluorad-FC 128" ® 2,2 "Lutensit AN 10" ® 20,0

Sodium trinitriloacetate 33.3

Sodium hydrogen carbonate 13.3

10 Citric acid 20, P

Polyvinylpyrrolidone 2.5

Diethanolamine 6.7

Polyethylene glycol 2.0

This product is prepared in the following way. 2 Kg of powdery Fluorad-FC 128 is mixed with 6.7 kg of diethanolamine and 20 kg of Lutensit AN 10 is added to the mixture. The entire mixture is then heated to 50 ° C and sprayed onto a pre-prepared powdered mixture of 33.3 kg of sodium trinitrile acetate, 13.3 kg of NaHCO 2 and 2 kg of polyvinylpyrrolidone to give a homogeneous, stable powder which is obtained in air cooled.

Then 2.0 kg of polyethylene glycol is heated and melted and sprayed on 20 kg of fine crystalline citric acid to obtain a powdered surface of which has been inactivated. This powder is then mixed with the above mixture containing the surfactants. This mixture can be used as such or it can be tableted or filled into capsules, bottles, pouches, packets or pads to form appropriate dosage units.

A dirty car, which was covered with a so-called traffic layer, which is difficult and sometimes not at all removable by cleaning under high pressure in the usual way, is washed under high pressure using the product according to the invention resulting in a surprisingly clean car that is freed from the said traffic layer.

The efficacy of a 13.5 g tablet made in this way is very good. The tablet has excellent mechanical strength, but it decomposes easily in water.

8203840 7

For comparison, it can be mentioned that the activity of a corresponding tablet, which does not include fluorine-containing surfactants, has an activity only 1-20 times greater. In order to obtain the same effect with that tablet as with the 5-tablet according to this example, it will therefore be necessary to use a known tablet which is approximately 20 times larger, i.e. a tablet of approximately 290 g.

As a result, the mixture according to the invention opens up new fields of application, for example for cleaning under high pressure, where it has hitherto not been practically possible to supply the detergent mixture in the form of tablets.

Example 2

A slow dissolving detergent mixture for car washing is prepared from the following components: 15 Components, parts by weight "Fluorad-FC 128" ® 2.2 "Lutensit AN 10" ® '20.0

Sodium trinitrile acetate 33, 3

DiSthanolamine 6.7 20 Polyethylene glycol, molecular wt. 6,800 2.0

Nonylphenol (30 mol E.O.) 35.8

This product is prepared in the following manner;

First 2 kg of powdered Fluorad-FC 128 is mixed with 6.7 kg of diethanolamine and 20 kg of Lutensit AN 10 are added to this mixture.

The resulting mixture is then heated to 50 ° C and sprayed onto 33 β kg of sodium trinitriloacetate powder. Then 2.0 kg of polyethylene glycol is heated together with 8 kg of nonylphenol (30 mol E.O.) and melted. The latter mixture is then finely sprayed onto the powder obtained above. The completely mixed product is then tableted to form 30 cylindrical tablets. Such a tablet is very suitable for use in high-pressure cleaning devices, without the need for tanks for chemicals and without a separate mixing device.

By using such a tablet, a higher pressure can be achieved with the cleaning device under high pressure, because no pressure drop occurs above the injector, while no chemicals are passed through the pump, and therefore not either. by the machine. The tablet according to the invention is intended to be placed in the washing tube, which is placed on the machine. In this way it is possible to keep the components of the tablet separate from the equipment thereby reducing corrosion.

Example 3

A neutral general purpose cleaning mixture is prepared with the following compositions

No. Components weight 10 1 "Fluorad-FC 170 C" ® 0 * 6 2 "Fluorad-FC 430" ® 1/6 3 Ethoxylated tridecyl alcohol (7 mol Ξ.Ο.) 2 £ 5 4 Ethoxylated tridecyl alcohol 15 (10 mol EO ) 3t0 5 Sodium trinitriloacetate 5.8 6 Sodium hydrogen carbonate 6 * 5 7 Trinitriloacetic acid Sc6 8 Po ly carbonz hr 2 .0 20 9 C12 ~ C14 diathano3-aid6 3 £ 0 10 Sodium tripolyphosphate 2

Components 1 - 4 and 9 are mixed together and then sprayed on a previously prepared powdered mixture of components 5, 6, 8 and 10 which is kept in regular motion and the resulting mixture is allowed to stand for half an hour; component 7 is then incorporated and the mixture is then left overnight. The product is then processed into dosage units, for example by tabletting. The entire procedure is carried out with the exclusion of moisture. Such tablets are suitable for degreasing methods.

30 Example 4

An alkaline detergent for dirty work is prepared from the following mixture: 8203840 9

No. Components parts by weight 1 "Fluorad-FC 170 C" ® 3.0 2 Ethoxylated tridecyl alcohol (10 mol E.O.) 15.0 5 3 Sodium tripolyphosphate 20.0 4 Polycarboxylic acid Na salt 3.0 5 Ξ0Ξ 66.0

Analogous to Example 3, components 1 and 2 are mixed together and the resulting mixture is then sprayed onto a pre-prepared powdered mixture of components 3-5. Finally, the obtained mixture is formed into dosage units, for example by tabletting . Such tablets are particularly suitable for use in the food industry.

Example 5 A 15 g tablet, prepared as indicated in Example 3, is placed in a beaker, after which 1 liter of water is added. The undisturbed dissolution rate at different temperatures is shown in the following table: _Min_Ο 1 2_3_4_5_ 20 7 ° C% 0 17 37 60 85 100 45 ° C% 0 39 75 100 65 ° C% 0 57 100

The pH of the resulting solution is 7.1.

A 15 g tablet prepared as described in Example 4 has the following undisturbed dissolution rates z _ Min 0 1 2 3_4 5_6_7 7 ° C% O 8 44 50 65 80 96 100 45eC% 0 44 65 97 100 65 ° C% 0 47 98 100 30 The pH of the solution in this case is 12.6.

From the above it appears that tablets according to the 8203840 invention can have a high dissolution rate. For comparison, it can be noted that commercially sold tablets under the name "Splendo Sprinkler tablet" prepared according to Danish patent application 5503/79 require about 8-20 minutes for complete dissolution.

A tablet made according to example 3 and a tablet made according to example 4 are dissolved together in 1 liter of water. By using a dose of 6% of this cleaning solution in a high pressure cleaner for car washing, an excellent cleaning effect on cars is obtained. The car is then completely clean and freed from the 10 film created in traffic. After that, a soft white cloth can be ironed over the paint layer without discolouring.

Example 6

A wax-containing car wash liquid of the following composition is manufactured in the form of tablets: 15

No. Components parts 1 "Fluorad-FC 170 C" ® "0.2 2 Tridecyl alcohol (10 mol EO) 4.0 3 C12 ~ C14 (^ -®t * ianolam; ^ e 2.0 4 KSI was 8.0 20 5 NaHCO ^ 25 6 Sodium trinitriloacetate 9.0 7 Tridecyl alcohol (25 mol EO) 2.0 8 Trinitriloacetic acid 12.1

First, components 1, 2 and 3 are mixed together and heated to 90 ° C. Component 4 is then melted and incorporated into this mixture. The resulting hot liquid is distributed over a half hour to a mixture previously prepared by mixing components 5, 6, 7 and 8. After that, the whole is pressed into tablets. A washing tablet weighing 15 g, obtained in this way, is placed in a beaker, after which 1 liter of water at 0 ° C is added. The pH of the solution obtained after dissolving is 7.5.

It appears that the tablet readily dissolves in the hot water, forming a completely homogeneous wash suspension, which forms an excellent wax layer when used.

Since many other embodiments of the present invention are possible 8203840 11 without departing from the rationale, it will be appreciated that all of the embodiments listed herein are intended only as an illustration and not as a limitation of the invention.

8203840

Claims (10)

Dosage unit for a detergent containing surfactants and additives suitable for the intended purpose, characterized in that the detergent contains a mixture of surfactants, consisting of 0 - 99 99% by weight of conventional surfactants. active substances and 0.01 to 100% by weight of fluorine-containing surfactants which are compatible therewith and which may be anionic, nonionic, cationic and / or amphoteric. Dosage unit according to claim 1, characterized in that wax is present as an auxiliary substance. Dosage unit according to claim 1, characterized in that a textile softener is present as an auxiliary material. Dosage unit according to claims 1-3, characterized in that the fluorine-containing surfactants are selected from the fluorocarbon-containing surfactants with 4-20 carbon atoms in the fluorine-containing carbon chain with 7-25 fluorine atoms and surfactants with one of the formula £ - ViaiAV * '° ηΡ2η1ΐ® ¥' 20 CnP2n ± 1X 'C F0 + .CH X, and n 2n-1 2 4 C F_ + .CH.-SO-X, n 2n-l 64 2 in which, in the case of anionic surfactants X, -OH, -NR ^ R2, -NHR3, -NHCH ^ OOH, SO3 ~, -SH, -CSSH, R2PO4 ~, etc., in the case of nonionic surfactants X represents -N (R4) CO (OCH „CH.) (OCH, CH-) oc.hq, zzn J zn 4 y and - (0CHo-CH_) -OH, -CN, -SCN, etc. 2. 2. n and in the case of cationic surfactants X -NHC2H4 = (C2H_) 2s · Ϊ / wherein Y is preferably a halogen, and in the case of amphoteric surfactants X represents + 1 2 -NHC2H4N = (R R) C2H4COO etc. Dosage unit according to claims 1-4, characterized in that the surfactants are 30% surfactants and 70% fluorine-containing surface -active substances. Dosage unit according to claim 1, characterized * 5 comprising: 0.5 - 5 wt.% "Fluorad-FC 128"% 15 - 25 wt.% "Lutensit AN 10" ^ 30 40 wt.% Sodium nitrile acetate 10 - 20 wt.% NaHCO 4 10 15 - 30 wt.% Citric acid 2 - 5 wt.% Polyvinylpyrrolidone 5 - 10 wt.% DiSthanolamine and 1 - 3 wt.% Polyethylene glycol. 7. A method of manufacturing a dosage unit of a detergent containing surfactants and auxiliaries suitable for the intended purpose, characterized in that a mixture of 0 - 99.99% by weight is prepared with the exclusion of moisture. conventional surfactants and 0.01-100 wt.% of one or more mutually and compatible fluorine-containing surfactants, which may be anionic, nonionic, cationic and / or amphoteric and evenly distribute this mixture over a mixture of the selected adjuvants, such that the particles of the adjuvants are coated with a layer of the mixture of the surfactants and the thus stabilized powder is mixed with a powdered acid, the surface of which is inactivated and the resulting powder, if desired, tablets or fills in capsules, bottles, bags, packs or pads. 8. A method according to claim 7 for producing a slow-dissolving tablet, characterized in that a mixture of surfactants is used and this is distributed evenly over a mixture of slowly-water-dissolving auxiliaries while excluding moisture, so that those with the surfactant mixture is coated, then the coated mixture is pressed into a preferably elongated tablet. Use of a dosage unit according to claims 1 to 6 for preparing a dose of detergent solution. Use of a dosage unit according to claims 1-6 for the preparation of a detergent solution for high pressure cleaning. 8203840