DE1467564A1 - Process for the production of detergent tablets - Google Patents

Description

(US 213,116 and 213 117 Prio July 30, 1962-2444) Colgate-Palmolive Comp.

Hew York. KoY./V.St.A. Hamburg, July 18, 1963 Process for the production of detergent tablets "

The present invention relates to a method for Distribution of detergent tablets in the waeeer easily disintegrate and completely dissolve and one Have sufficient resistance not to break during transport or when falling.

It has been found that such detergent tablets can be used can produce by producing a finely divided detergent mixture with a high silicate content, this with Water was added and compressed under low pressure to form a tablet containing fora. It was also found that that the presence of oineo water-soluble sulfates in the Detergent mixture facilitates the preparation, compression and handling of the finely divided detergent mixture.

Accordingly, the invention provides a process for preparing serfallenden in ymasv easy wasserltioliohen WaschmittelSablafc th Torgoochlagen, which is characterized, d © 3, a finely divided Waschmlttel-

-2- ORIGINAL BATHROOM

909841/1396

mixture with a content of

2 to 20 pounds of non-katloniaohen eynthetiacheo organic washing raw material,

20 bia 50 i "water-Polypaoephat and _fc.

20 to 50 pounds waaaerlöaUchem Metallailikat

divided, with continued Durohmiechen bia to achieve a moisture content of 15 to 35 3 * old Waaetr offset and subsequently to form and under low pressure Bruohbeat-resistant tablets compacted.

The wax medium tablets compacted into tablets by the process according to the invention can, for example, contain up to 13 liters of wax before the waaaer addition . Contain water and a water-soluble metallic lattice with a metal oxide di 3iO ₂ ratio of 0.3 to 1.

According to another embodiment of the present invention

Detergent particles are also 2 to 20% cationic synthetic organic ffasohrobetoff, about 25 to 40 waaeerlösliohem i ° waeaerlOalichem Polyphoaphat, about 20 bia 50 ^ Metallallikat with a Vernültnia Motalloxyd 31o t ₂ of 0.3 to 0.6, about 4 bla 12 £ waaaerlOaliehern sulfate and up to 15 ^ water under continued mixing until a moisture content of 17 30 bia i> veraotzt with water and compressed under low pressure to form tablets.

-3-909841 / 1396

BATH ORIGINAL

U67564

The present invention extends calibration also to detergent tablets having a content of 2 20 1 * Ms washing base 25 Ws 40 * Polyphoephat, 20 to 50 + metal silicate, 3.5 to 10 water-soluble f sulfate and 17 to 30 l of water.

The non-cationic, synthetic organic washing pipe

Fabric is usually a niohtional laundry raw material, ¹ VDr assigned with both hydrophilic and hydrophobic

Groups in the molecule of which at least the hydrophilic part i

a plurality of interconnected alkylene oxide contains groups. A preferred washing raw material of this type are the alkylphenol polyalkylene glycol ethers. Nonylphenol poly ethylene glycol ether with 9 to 10 Xthylenoxydgruppen per

Molecule have been approved for use in accordance with the present Invention as an excellent, non-organic raw material

proven. Usually the alkyl group of the alkylphenols 6 to 14 carbon atoms and the polyalkylene glycol ethers chain 4 to 12 alkylene oxide units with 2 to 4 carbon βtoff contain atoms. Although the aforementioned

Phenol derivatives are of particular importance according to the invention

Mixtures of non-ionic Wasohrohstoffβ can also be used be used. So you can either alone if you wish or together with the alkyl benzene polyalkylene glycol ethers other non-ionic washing raw materials, for example Hlock

Copolymers of ethylene oxide and propylene oxide (Pluronioe), Reaction products of higher fatty alcohols with lower ones

909841/1336

SAD ORlGiNAi.

H67564

Alkylene oxides (Emulphogens), polyethylene oxide adducts of higher fatty acids (Emulphore), polyalkylene glycol esters and ethers and in particular polyethylene glycol esters and ethers of polyalcohols, in particular of sorbitol and mannitol (Spane, Sweons) can be used. Regardless of whether a single nonionic Wasohrohstoff or a mixture is used, the proportion based on the detergent tablet should be in the range of 2-20, preferably 5 to. 15 »in particular 6 to 14 $ · are all in the present specification and the appended claims mentioned percentages refer you Seetandteile _t unless otherwise specified, exceeds the weight of the tablet and therefore not Gesamtprozenteatz 100 #.

In addition, ZM the nonionic Wasohrohstoff can be used in the detergent tablets according to the invention instead of part of the nonionic. Waso raw material use an anionic wax raw material, usually mainly for tree strengthening and to increase the cleaning power. In some cases it is desirable to replace the non-ionic water raw material with a suitable anicnical product. Sodium alkylbenzenesulfonate and, in particular, sodium tridecylbenzenesulfonate are preferred as the anionic washing raw material. This material is made by the alkylation of benzene with a mixture

-5-909841 / 1396

BATH ORIGINAL

axis propylene tetramer and pentamer produced · Bio alkyl groups are heavily branched, but other alkyl groups with a relatively straight-chain configuration and 12 carbon atoms are also suitable. The anionisohen Wasohrohstoffe are generally used in the form of their water-soluble sodium salts, but other water-soluble salts, for example alkali salts, in particular potassium salts, can usually be used instead of part of the sodium salt. Instead of alkylarylsulfonates, other anionic organic wax raw materials of the sulfate or sulfonate type can be used. Examples of these are sodium lauryl sulfate, sodium monoglyceride sulfate of coconut oil fatty acids and sodium salts of higher fatty acid amides of N-methyltaurine. These compounds contain a fatty alcohol or fatty acid group with 10 to 18 carbon atoms as a lipophilic component and are used in the form of their water-soluble salts, preferably their alkali salts. The content of anionic detergent raw material complements the content of nonionic detergent raw material, so that the sum of the two contents, based on the detergent tablet, does not exceed about 20 μl and not below about 2 μl .

The water-soluble metal silicate has the unusual effect in the waachraltteltablette according to the invention Applying only a slight pressure results in the formation of a

• 6-909841 / 1396

shape-retaining and break-resistant tablets, which nevertheless fall quickly in the aqueous medium and completely dissolve in a short time. Silicates make it possible to produce tablets with a low bulk density and do not require the tablets to be coated · Among the silicates determined to be suitable, the particular ones are · alkali silicates, a special itodium silicate · with a weight ratio of metal oxide 31O ₉ of about 0.3

up to 1, preferably 0.3 to 0.6 used »Particularly preferred * Sodium silicate with a Na ₂ O t ratio of 1 t 2.35 is added. However, you can find out more about the invention. Tablets to achieve similar effects, other silicates of the general type described can be used either instead of or together with the preferred silicate.

The water-soluble polyphosphate is a metal salt, usually an alkali salt, and preferably the sodium salt a polyphosphoric acid. Particularly preferred among these salts are pentanesodium tripolyphosphate and tetrasodium pyrophosphate. Instead of or in a mixture with the sodium polyphosphates mentioned, according to the invention, auoh Other polyphosphates with a satisfactory Waachalkallenffekt be used, as far as they are used in the production of Allow tablets. Depending on the desired properties of the end product, either the sodium or potassium salts of these substances are used »

-7-909841 / 1396

Dae in the detergent particles to be moistened, possibly in addition to the other washing raw materials and washing agents existing water-soluble sulfate improves the processing properties significantly. An inorganic β sulfate, especially a metal salt, is usually used Sodium sulphate is particularly preferred, but other alkali sulphates, for example potassium sulphate, are also used as long as they show the same general effect in the misohung.

Aueser contain the deatand parts mentioned above

the finished tablets water · Furthermore, can be used to achieve Particularly desirable properties the detergent tablets further auxiliaries are added · to these Fabrics include other Waecha! Italy, sound amplifiers or β ν anti-haze agents, dyes, perfumes, bleaches, medium, solvents, fluorescent dyes, settling preventive agents and the like. To an impairment | the beneficial physical properties of the Avoiding bulk tablets should only be a low one Total amount of excipients to be used.

In order to achieve the economic and efficient production of a product with satisfactory features and functionality to ensure the proportions of

-.8-909841 / 1-396 bad or.cnal

non-cationic Wasohrohstoff, silicate, polyphosphate _t Waoaer and possibly sulphate are within the framework set out in the following descriptions .

The amount of oynthetisshen organigehen washing raw materials aoll in the range of 2 to 20 # are "preferably 5 Ms $ 15 and" γοη in the presence of sulfate in particular 6 l) is $ 14. It has been found _s that such a content of organic Waschrohetoff in conjunction with the Silicate and the phosphate of the tablet gives excellent cleaning properties, which allows the production of a wiüntandQ ~ capable and yet dissolving detergent tablet '«} enables detergent tablets with a gelatinous raw material below the limit have no satisfactory qualification, honoring higher proportions sn TVaeclirobgtoffon may hit the desired properties of the leaf niolite tercinl5f ...

jic phosphate is said to B>"hi.® jo $ _{ , wise 25 Mo 40 # w / rr.5." in particular 30 f & qt (Dalüette mm ™ iaaoheric An utterly ripped Phoepliat ^ alialt 'forlaibt around Iroüiik excellent VtemGhtiVmli en- miss. Iiof .nlgaugssigOngOhnf f mx beef -antGTtiMktxt (Ims 81 Xi! rat tmi dei «He ^ r-- '- ^ ittng einer rioh rage !! nufl« «saij, ien! Fe'tflsite alt f.ns and Atx ·! .plwimnW , iili ^ Q * ^J < _β M-- m Ή- · ?. ^ n

f ^7. ^: · π aa- * eh «inen Τ ^ ΧΆίη * vr-vlianüsnen

909841/1396

Water can be completely hydrated, @o that some of the water remains to make the silicates more easily soluble in the Wasohwaaser _o

The water-soluble silicate content of the tablets is 20 to 50%. It has been found that this amount of silicate is worthwhile in order to achieve a rapidly dissolving product with excellent resistance to corrosion, in honor of normal transport. The preferred amount of silicate is 20 to 40 #. Sin silicate content of the erflnducgagsmälen detergent tablet within this Mo ^ genverhältnisse bawirkt a profound Yerändaruug represents tablets own sheep ton "The tablets are easier to keep and Doueh solid _f dia particles angar zmsmmn ,, so that dia Bruchneigttng at rnivoicsicihtiger Bshandlung sarüclrgeJit ai; ö the tablet ifiä-t aieh still very warden TSLdQh © uf _e Diesa advantageous Ei'gtbnisae ^ without the detergent tablets © inen top. (

The water content contained in the detergent trays is essential for the syrup of a product with the above-mentioned proprietary sobaftan. Bas water causes a complete or in some cases complete hydration doa Folyphoaphats and yarbeaaert considerably the Löolichkelt of the silicate, so that after the introduction of the

-10- 909841/1396

BATH

Detergent tablets in the washing water practically no insoluble grains remain. The water content of the tablet should be 15 to 35 · 1, and preferably 20 to 30 i ', so that a substantial hydration, that is, a hydration of 75 ί> or more of the polyphosphates is carried out. In the presence of sulphate this is used to achieve this. Results a water content of the tablets 17-30 i> and in particular 19 preferably up to 25 #, where a considerable "Liehe enters hydration. The the detergent zügatiatzle amount of water is 2 to 35 #, preferably 7 to 30 i» and in the presence of sulfate preferably 2 to 30 %, in particular 7 to 17%. It has been found that, within the limits specified above, more water can be incorporated in the detergent table tier if silicates with a lower Na ₂ O 3 ratio of 0, 3 to 1.0 and preferably 0.3 to 0.6 can be used.

s

In order to achieve improved processing properties, the detergent tablets advantageously contain 3.5 to 10 $> sodium sulfate * Such a content can be achieved by producing detergent particles with a content of about 4 to 12 J * sodium sulfate, with the addition of

Water caused a reduction in the percentage of sodium

sulfate is balanced, "

-11-

909841/1396

With regard to the other components of the washing tablets according to the invention, the same percentages were given both for the finished tablet and for the detergent particles used for their production, in order not to unnecessarily complicate the understanding by citing further quantitative ranges for the detergent particles. However, it is expressly pointed out that the specified areas essentially describe the finished product and the similar

The composition of the mixture in the mixer and the ingredients are selected accordingly. It was established that the mixing and agitation of the mass quo can be interrupted for up to an hour if the product, based on the detergent tablet, is 3? 5 to 10 # "Preferably contains about 7 ¥> sodium sulphate" If necessary, the microprocessor can be interrupted without further ado or the material can be kept for compacting without adding the already pretreated washing raw material organize effective production iUS _t since ess no longer necessary _r iat the Durchsatzgeschwinäigkeit the compression stage of the ZuführoiigJigeschwlnälskeit A ~ aatzproättktes from Sprllhturm to Beieuohtungavorrichturg precisely match

«12- 909841/1396

For the production of the detergent tablets according to the invention, wax tablets are produced which contain the organic detergent raw material, the sulfate, the silicate and the polyphosphate. It is highly preferred that the constituents of the detergent mixture within? the particles are homogeneously distributed. Detergent pearls produced by spray drying have proven to be an excellent starting material for the production of the tablets. For complete drying, a solution or slurry of the raw washing materials in an aqueous medium is used, with this so-called "soap scrubbing product" being added suitable additives that are not affected by the spray drying "A watery dispersion or solution normally has a solids content of about 40 to 60 $ ₉ and is sprayed through spray nozzles and dried by heated gas during the fall * The collected particles can be cooled, sieved and classified" in order to separate out undesirably large or small particles "The product obtained may contain certain irregular shapes, but generally consists of approximately spherical hollow particles. For conversion into the detergent trays according to the invention, those products are suitable which have a grain size of about 0.1 5 mm to 2.4 mm. Most of the water present is removed during the drying process, but the partial claws usually still contain at least 1 $ and up to 15 ^ and in particular up to 13 # * euohtisK * U, 9098A1 / 1396

BAD ORiGiNAL

The homogeneous detergent particles can also after other Process than can be produced by spray drying. For this come * see B. Spray cooling, agglomeration, uniform Milling and subsequent sieving and classification into Ss can also be part of the product spray-dried and separated with organic wax, silicate and phosphate are added. However, it is essential that a substantial tail of the existing silicate, at least about 75 #, ßo as with a spray dried Product along with the phosphate and the organic Wasthrohstoff equalis & eslg through each of the particles is distributed.

The detergent particles described above with high Silikatgekalt be, for example, sprayed in a drum mixer with continued movement with water in the form of fine droplets so that the final product has a moisture content of 15 to 35 i '% preferably 20 to 30 ° i. The continuously agitated and mixed particles can easily adhere to a number of other particles during spraying and mixing. Prior to wetting, the detergent particles have an apparent density of about 0.2 to 0.6 g / cm o as a result of wetting this density changed somewhat, usually decreased by as much as $ 30. This is due to the wetting of the relatively large proportions of silicate and

-H-

909841/1396

ORIGINAL BATHROOM

^τ 1Λ67564

^: _ 14 - ■ ■

uiiä Poljphosphafc and the sources resulting from it of the substances with increase in particle size traced back.

There is adequate and even moistening of the detergent Holds particles or food with a high silica content dae silicate in ainar easily soluble form, 30 that on no undissolved silicate deposits on the washed parts

"Gen zurückbleibenο Bio® is τοη importance for the Waschmittslcheaalksr because iuo silicates tend dasu, the Br ^ rms for expelling the adhering moisture, sis, for example, in spray drying, unlBsIlcher su w © rden _o Aueli the PoljFPhöophate attract vox'augswalse Peuchtigkeit and often tend dae silicate in a wenigsr lös heights SSratima su iibertUhrena self bai Vorhanäenaein .One-üborechussee won Waessi ^1, wi © beiapi as wise kömien in Vaschmaschiney .derartige silicates not see uittei * uiaständen Ehrend ä & a fully Waschvorgangee

dissolve and then list su atSran & cm deposits the washed rushes <> Bsi den © rfintlurg, according to laughter Tablets are due to the relatively high concentration the 3il.ikatl8ung obtained when moistening the air with a high silicate content with any silicate lower solubility made soluble quickly «Dios @ more soluble The shape remains after being moistened for a long time « hold and the tablets made from it are still Month after your®? Manufacture completely soluble.

-15- 90984Ί / 139β

BATH ORIGINAL

afc <(£ <»

If the material to be moistened is constantly kept in and the moisture is brought into the Porm von TrUpfohon ;, eo an extremely even distribution of the moisture content in the washing raw material without undesired agglomeration is observed. After the mixing, lighting and agglomeration to a desired ®s * level , the compressed washing raw material can be sieved to the desired grain size. A particle size between about Of4 and mm has also proven to be advantageous, "

however, other size ranges can also be used; will. 13a is generally more difficult to eat large amounts of moisture within the specified limits.

set when detergent with © ehr low-lying AnfaiigßfetKshtigkeit venvenS ^ tt 3rd "n _o When the particles initially verbÄltnieHäi3i.g?; trcclicn are is usually en ^ _t anachenewert more than Torgeeohrie-bene MindeiitEcnge of moisture ausübet; sen ο The Elnaeliisi t ^ rj of the Miaciivsrfahren _t for example its speed ι

and duration karmen.in dependence on dar Miec> iYOi * rioh1? Ang; be easily gsrßgelt so that the Wagefcaaitteltallein be moistened in the esa ööeten suitable manner ;, may & ^uqü: a two-stage addition of Waoser ^ Jsacheiißwort seiiig wherein initially a certain Wasaeroange give .and. the Miechung hinreichsnäs 2eit _t big 5 30 minute gemiajlit and then another is added. In “this way, one can dig into the middle particles

9098 ^ 1/1396

U67564

bring in and still an excellent, well-deserved cash Material received. As already mentioned, the speed can and the duration of the mixing for the purpose is regulated

■ *

is ,, however, has a measured at the circumference of a drum provided with inner guide surfaces of Mieehgeschwindigkeit ₉ O 5 and 1 * 25 m / sec. proved suitable. Appropriately moistened detergent particles can be obtained in a mixing time of just 1 minute »

In the presence of sulphate in the mixture, the moistened product is not susceptible to the formation of undesired lumps or coherent masses * The moistened detergent particles can be stored for up to an hour and in some cases even longer and are then still free-flowing and suitable for transport to the presses. The reason for this highly unexpected effect of this specific amount of sulfate is not known. Theoretically, one can assume that sulfate interferes with the hydration process “regulates the rate of hydration of the other salts and thereby changes the type of aggregate produced. Mixing or tablets should be used to achieve the appropriate product. ,. be carried out continuously and with at most momentary interruptions ο

909841/1396 ^ßAD

When the silicate-containing detergents are moistened, they are pressed into a desired shape under slight pressure. Any suitable low pressure can be used to produce the tablets © about 2 paw 2.5 cm thick is "to use a pressure of about Q ₉ ^ to 1 _-9 8 kg / cm." Pressures above 7 kg / cm should be avoided carried out, the surfaces and cavities of which are chrome-plated ο ed fe Teflon coated ο It is not necessary to "subject the pressed! product to a special post-treatment or aging process before transport, although it is important within an hour after the extinguishing process" -Feetigkeltsstdlgerung

Dia WSetachmltteltablefeten beeitzan sufficient

To Sen Transfnrt Without Breaking Or Serious A

zn over and can be known at any ©

be packed »The inventive

iiabön h & xätig © ine -wünechonswarte low density, - so

As a result of their larger volume, they can be used by consumers and are in the event of a loss

Obtained untsi-part m & aQn k @ nnen- ₉ -, yowait © ine

Control Waschml is used t telkonzontration important appears "

41/13 9 6 ORIGINAL BATHROOM

33a according to previous observations it was to be assumed that the addition of sulfates increases the density of the products, it was by no means to be predicted ₉ that the detergent tablets according to the invention and the corresponding detergent powder have the desired low bulk density of 0.2 to 0.6 gfowr , surprisingly these light tablets are also more resistant than comparable tablets made of heavier materials with a lower silicate content. The tablets according to the invention can be produced by a more efficient process using tabletting devices of conventional design. Sa the date as necessary and still door many other detergent tablets unnecessary deemed substantial * coating _s iet the speed and effectiveness d © r Hersteilung be increased "All these advantages are achieved without it being necessary to Waschronetoffen relatively expensive for conditioning Adding auxiliary substances

Although it used to produce a satisfactory Product is unnecessary, the invention-appropriate Wasctamltteltabletten to provide a coating, you can dia Tablets on Wunsoh on the surface with moisture spray ο In special cases you can of course use the Tablets with a thin film of an organic polymer for example from ITatriumcarboxymethylc ellulo se or. Polyvinyl alcohol added to harden them even further

909841/1396 ~ ¹⁹ ~

BAD ORIGJNAL

and make up unusually rough treatment resistant · Per specialist will be other possible variations dee erfindungegemäßen process recognize _f However, the present invention provides a useful product and changes in the method of production are in custody not required, but may sometimes be desirable, "In some cases, the Moisturizing solution does not contain heat-stable auxiliary substances, for example emulsified perfumes. A little sodium particulate can also be added with this solution. The manufactured products can subsequently be perfumed, colored, provided with a coating and packaged for transport. It is preferred to pack the tablets in watertight envelopes, for example aue polyethylene film, but they are still break-resistant and easily soluble even after months of storage in the atmosphere »

The detergent tablets produced by the process according to the invention were tested under harsh conditions and, after aging, a tablet usually withstands at least impacts equivalent to five drops from a height of about 1.20 m on a hard floor before it begins to break ". The tablets aeigen also after packaging in Polyäthylenhttllen despite repeated shaking of the package in _s approximately corresponding to a careless hand elevation during transport, no disturbing abrasions

-20-909841 / 1396

BAD ORIGJNAL

. - 20 ~

Despite their great strength, the tablets dissolve., smoke and completely and usually completely disintegrate within 45 seconds and mostly within from 10 to 30 seconds ».

The following examples serve to explain the embodiments of the process according to the invention and the products manufactured therefrom »The invention is not to the embodiments described in the examples limited «Unless otherwise stated, all information on quantities and proportions are weight

declarations"

Example 1 ,

In a Seif enmi shear "an aqueous mixture was formed with a solids content of about 55 i> from those listed in the following constituents with the exception of the pigments.

Parts by weight

Nonylphenol polyethyl glycol ether with an average of 9.5 ethylene oxide groups per molecule 10.0

Sodium tripolyphosphate

(including the Piioephatpro-

drying products from spray) - 30.7

Sodium silicate

(Na ₂ O a SlO ₂ m 1 j. 2 "35) 30.3

Sodium sulfate 6.6

Sodium cerboxyethyl cellulose 0.4

Auxiliary materials (pigment ,, PluoresEenss- »fbfi ⁾

^Wae8ar

BAD ORIGJNAL

The resulting mixture was aged eingeeprttht a temperature of 57 ⁰ C under a pressure of about 21 kg / cm in hot Trocknungsgaa with a Anfangetemperatur of about 316 ⁰ O. The particles obtained with a particle size of about 0.15 US 2.4 mm had a moisture content of about 10 $ and were circulated in a slightly inclined drum mixer rotating at a peripheral speed of about 0.5 to 1.25 m / sec and sprayed with finely divided water. The sprayed product was continuously drawn off with a moisture content of 21%, sieved to a grain size of about 0.4 to 4.8 mm and pressed after storage for a maximum of one hour. This product can still be pressed after several hours and does not show any on storage disturbing lump formation.

Before compression, the product has a bulk density of about 0.25 g / csr and the spray dried product one Bulk density of about 0.3 g / cnr. The product becomes a flat, rounded cylindrical tablet with a diameter of 6.35 cm and a thickness of 2.07 cm, a weight of 37 g and a bulk density of about 0.5 g / cm ^ pressed to The pressing pressure was about 0.3 to 1.8 kg / cm.

The tablet obtained was an excellent detergent, and quickly disintegrated in the wash water in a normal washing machine · The tablet did not break when immediately

. ; -22 «

909841/1398

- 22 -

fell on one of its edges from a height of 60 cm after manufacture. The strength of the tablet took after several hours of aging or after drying 2-5 i> sprayed onto the surface moisture or to ". .

Example 2 .

Ea a detergent tablet was made with fblgendar Composition ι Components » parts by weight χ

Nonylphenol polyethylene glycol ethers with an average of 9t5 ethylene *. οxya groups per molecule

Sodium tripolyphosphate, anhydrous

Sodium silicate, based on solids (Na ₂ O % SiO ₂ «1 ι 2.35) - water

Perfume, dyes, other additives

100.0

To produce the tablets, the non-ionic detergent raw material, the sodium tripolyphosphate, the sodium silicate and the dyes were mixed in a soap mixer to form a uniform aqueous slurry with a Feetatoff content of about $ 50 and then spray-dried in a drying gas in a conventional spray-drying gas usual bead shape and was sieved to a particle size of 0.15 to 2 »4 mm. The moisture content of the product obtained was about 8 °

9098 * 1/1396

9 .4 • 7 28 , 9 33.4 27 t 0

The spray dried product was in a suitable MiBeher, for example a slightly inclined drum mixer, circulated and used. uniform humidification a moisture content of about 28 # with small water * droplets sprayed. Bas ParfUm was sprayed on just before moistening. After continued stirring to the The bulk density of the product of about supported an even distribution of the moisture 0.4 to 0.3 decreased This «product became about Compressed 22.5 mm thick tablets with a diameter of 64 mm and a weight of 42 g “For the production of Tablet bit of uniform thickness was applied Pressure through a fixed stop device controlled · The pressure effectively exerted on the tablets was in the range of about 0.2 to 1.8 kg / cm «

The tablets obtained had excellent cleaning properties, disintegrated quickly in water and were extremely resistant to breakage and abrasion. The tablets loading "were required for commercial use HRR th and disintegrated still in cold or hot, he shall _r without HUhren, _o within seconds von.30 Some of the tablets disintegrated in just 10 seconds. The unusually rapid disintegration and accompanying dissolution is at least partly due to the rapid removal of calibration-dissolving tablet material, which

-24 -90 9 841/139 6 u

descends from the floating red part of the tablet ... The tablets did not disintegrate into lumps in the washing water, but dissolved quickly and regularly. «The tablet did not break when dropped several times from a height of 1.20 m. In the washing machine could synthetic Soiled tissues are effectively washed with these tablets and compared to those currently on the market located ha: Adele usual tablets with a lower Weight of. lighter tablet can be cleaned and made completely white again «. Bie.Waoh effect the invented tablets corresponded to a lot - ' commercial, synthetic ßrobwaeehmittel, which a higher proportion of organic washing raw material and Natriuratripolyphoaphat contain

Colored detergent tablets according to the invention with a content of blue-coloring substances which adversely affect the fabric; en _f ^ iQxui the tablet can be used for sufficient time without the risk of discoloration of the gev / asohunen parts due to the rapid dissolution of the tablet in the washing water. This is aurUckzuführen dareaf that the tablet disintegrated, dissolved and distributed calibrated before could be adsorbed by the Textilfeaern a stBrende coloring or retained ₀

: '-25-

909841/1396

BATH ORIGINAL

U67564

Example 3

Following the procedure of Example 1, detergent tablets were made produced with the following composition

Component Weight part Nonylpheiwlpfrlyäthylenglykoläther
with an average of 9.5 ethylene
oxide groups per molecule 10.4 Sodium polyphosphate 32.3 Natriuraailikat
(Na ₂ O ι SiO ₂ · 1 -t 2.35) 31.6 Sodium sulfate 3.5 water 21.0 Help 1 _f 2

100.0

After the pre-compression, the! Tablets were given 2 to 5 # Water sprayed and quickly dried

The product obtained was a satisfactory detergent, exhibited high resistance to breakage, and very quickly disintegrated in the washing water when placed in a washing machine. Until Afo ^ iabsbeatigkeitksit was very high _p üeilweis as a result of the aftertreatment with water o The moistened detergent particles used for the production of these tablets did not form lumps and were mobile enough to be transported from one processing device to another even after one and a half hours of resting aging » In this respect, the product was considerably superior to a similar product without sulphate content »

909841/1396 ~ ²⁶ ~

BATH

'- 26 -

Example 4

According to Belepiel 3, the following components were made a detergent tablet made! .

Components! parts by weight

Nonylphenol polyethylene glycol ether with an average of 9.5 xylene oxide groups 10.0 per molecule

Sodium tripolyphophate (incl Phosphate products from spray

drying) 40.0

™ sodium silicate

(Na ₂ O ι SiO ₂ * 1 Ί 2.35) sodium sulfate

Auxiliaries (pigment, fluorescent "dyes, perfumes, inert auxiliaries)

water

100.0

The product obtained is suitable as a detergent tablet, although the detergent particles produced are higher Have bulk density than those produced using a higher silicate content »This effect can partly on the spray properties of the soap mixer product and the following differences in humidification effects. Bie Waachmltteltellchen were easy to work with, showed no annoying lump formation or "sluggishness" after standing «,

-27 »

20th "O 8th fO 1 , 0 21

909841/1396

A detergent tablet was prepared according to Example 3, but now the 3.5 parts of sodium sulfate. was replaced by a 10 file and the moisture content was changed to _o The product obtained corresponded to Example 2, was easy to process and showed no sluggishness.

6 - IO

Following the procedure of Example 2, detergent tablets were made with the addition compiled in Table 1 sainmenaetiung made;

Table 1 Meh-featgilei
. ■ &. "Vol .; 8.6. 1P " Components «. Ge 11.0 14.0 Nonylphenolpoiy & Thyienglykol-
fither with German technical
9.5 xthylenoacyd groups per
Molecule ■ '■ - ■. -JO ₈ O 11.3 «V _ Sodium Trldecylbonjüolflulfonat
(8o $> detergent substance) 3318 26.0 27.6 Sodium trypolyphoid 30.7 34.8 33.2 27 »2 Sodium silicate
Solids)
Na ₂ O ι ISiO ₂ * .1 s 2.35 30.2 .- - Na ₂ O a * SiO ₃ «1 ε 1.6 - 34.3 - 2.7 18 "O Na ₂ O t iÜOg «» tti -'-. · ■. - 3.5 ma Natrlumh ^ droxyd * - -

Auxiliary materials (,

blue, brightener, aaaetzverhti-

tend substances) 1.2-1.4 1.4 1.0 1 "1

M & Ig *? 1? «1 gif2 17.0 100.0 i6ö, ö 100.0 IW ^ iöo» o

-28-09841 / 139 6

U67564.

The dimensions of the tablets obtained corresponded to those of Example 2 and weighed from 37 to 46 g. The tablets showed a good rate of release in water, good resistance to breakage when dropped, good abrasion resistance and excellent cleaning and whitening effect · The tablets could be repeated without crime. from a height of 30 cm to 1.20 m to be dropped «juices disintegrated in water within 10 to 30 seconds and showed after shaking in one Enclosure made of plastic film no disruptive abrasion. The products were special in all of the above suitable for use as a detergent '

Example 11

By the method of Example 2, detergent tablets were prepared with the following composition%

Constituent . Weight s

Nonylphenol polyethylene glycol ether
with an average of 9.5 ethylene oxide groups per molecule 10.0

Sodium polyphosphate 30.7

Sodium silicate

(Na ₂ O 8 SiO ₂ - 1 s 2.35 30.3

Water 21.0

Auxiliaries (perfume, dyes,
Fluorescent brighteners, inert auxiliaries

-29 «

90 9841/139 6

You moistened detergent were applied to a particle size of 0.4 to 4.8 mm sieved "Naoh the pre-pressing at low pressure were the tablets wetted on the surface with 3 $> water and dried up the water * Bas product obtained was with the exception of minor Quantities of dispersible pigments and inert substances completely soluble in water, disintegrated within to 30 seconds, with a breaking force of about 9 to 14 kg applied 12 hours after production and was a satisfactory detergent usable detergent tablet can be produced. However, it is preferred to divide a tablet with a particularly high strength by moistening it with about 2 to 5 fi water and then drying it. "

sto s eu <

909841/1396

Claims (1)

JU (VtB 213.116 and 213 117 Colgate-PalmoliYe Co "p. ^M * * *** ^ ² - ² Hew York "y" Y./T "£ ft" A, _T Hamburg, $ 1 · July 1963 Fate ntana claims. 1. Process aur production of water-soluble detergent tablets which disintegrate easily in water, characterized in that a finely divided Waachmittelmlachtmg alt a content of 2 to 20 %> Non-cationic, synthetic organic detergent raw material 20 to 50 i> water-soluble polyphosphate and 20 to 50 <£ water-soluble «metal silicate produced under continued Burohmlaohen until a moisture content of 15 to 35 £ is reached with water and then under low pressure to be dimensionally stable and break-resistant Compressed tablets. 2ο method according to claim 1, characterized in that dafi one f one-part detergent mixture with a Salary of 3 to 15 t washing raw material, g 25 to 40 i> metal silicate with a ratio UD never Hetalloxyd s SiO ₂ from 0.3 to oo. and . ^ 0 to 13 S * water ^ with continued mixing until it is reached cn a moisture content as of 20 to 30 % with water ▼ replaced and compressed into tablets » -2- OMGtHAL INSPECTED 3. The method according to claim 1 »characterized in that nan an aqueous Waecnmittelmlechung by spray drying in
5 to 15 i> lower polyalkylene glycol ethers, 20 to 50 $> water-soluble tripolyphosphate, 20 to 50? S water-soluble alkali silicate and 15 to 55 # water particles enthalitende detergent überfuhrt "these and shatter resistant until reaching a moisture content ** 19-25 $> less with water in the form of droplets was added with continued mixing and subsequently under a pressure of about 0.2 to form- to 1.8 kg / cm Compressed tablets with a bulk density of about 0.3 to 0.5 g / cm ^. ' 4 · A method according to claim 1 to 3, characterized in that 4 to 12 $> water-soluble sulphate at ₉ preferably Alkalieulf and up to 15 water-containing wash # * "mittelteilchen with continued through slots to. * to achieve a moisture content of up to 30 wt. ^ mixed with water «, cd 5o method according to claim 3t characterized _p that ^ you can mix an aqueous detergent mixture by spray drying _, nung .in ^ 6 to 14 ί> polyethylene glycol ethers ^ J 20 to 40 Jt sodium silicate with a ratio cd Na «0 j SiO ₂ of 0.3 to 0.6,, cn 4 Mo 12 Ji sodium sulfate and $ 8 to $ 12> Waeaer containing ingredient particles transferred BAD ORIGiNAU 6, Wasohaitteltablette, which is dimensionally stable and break-resistant, easily disintegrating and dissolving in the waeaer, thereby characterized in that the tablet of low pressure compacted detergent particles with a Salary of 2 is called 20 # non-cationic synthetic organic waso raw material, 20 to 50 f water-soluble polyphosphate, 20 to 50 $> water-soluble metal silicate and. $ 15 to $ 35> water exists o 7 * detergent tablet according to claim 6, characterized in that the tablet is made from under a pressure of ' A maximum of 7 kg / cm of compacted detergent parts with a content of 5 to 15 i * higher alkylphenol polyalkylene glycol ether, 25 to 40 i> water-soluble tripolyphosphate, From 20 to 40 $> WAO β redeeming Ii ch em metal silicate having a ratio of metal oxide SiO t ₉ -from 0.3 to 1 and. * 15 to 35 ί » water and a bulk density of 0.3 to 0.5 g / cnr owns. ο detergent tablet according to claim 7, characterized in that the tablet consists of detergent particles compacted under a pressure of about 0.2 to 1 “3 kg / cm ² with a content of -4-909841 / 1396 ' BATH ORIGINAL "14b / SbA β to Η- $> Nonylphenolpolyäthyleiiglykolä '& her with 9 to 10 Ithylsnöxjägruppon per molecule $ 25 to $ 40> Sodium Tripolyphosis Frai, 20 to 40 36 rratriurasi-silicate with elnom VerhOlfenis Na ₀ O s SiO «τοπ about 0-, 4 u 19 to 25 $ water
there, 9ο Vaechmittsltablotta according to Äiispruish β to 8 ₉ gokennaeleh nat with a content of 3.5-10 $> waoaör3.! Islteh © »i sulfate; ο ! au BAD ORiGJNAL 909841/1396