Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/04—Water-soluble compounds
  • C11D3/08—Silicates
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0047—Detergents in the form of bars or tablets
  • C11D17/0052—Cast detergent compositions
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0047—Detergents in the form of bars or tablets
  • C11D17/0065—Solid detergents containing builders
  • C11D17/0073—Tablets
  • C11D17/0078—Multilayered tablets
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/04—Water-soluble compounds
  • C11D3/06—Phosphates, including polyphosphates

Definitions

• the invention relates to detergent compactates, in particular for the automatic cleaning of dishes, a method for producing the detergent compact and the use of these compactates in the automatic pre-washing and cleaning process of household dishwashers.
• the priority German patent application P (D 7294) describes detergents in the form of a melting block, in particular for the machine cleaning of dishes, which are in the form of multilayer structures, the individual layers having a different dissolution rate in the mechanically predetermined time-temperature curve. As a result, one layer should dissolve in the cold water of the pre-rinse cycle, another only with increasing water temperature in the wash cycle.
• German patent application P (D 7316), which is also of the same priority, describes multilayer detergent tablets for automatic dishwashing, the composition and application of which comply with the same principles as set out above.
• the cold water-soluble enamel layer for the pre-rinse cycle consists of cold water-soluble alkali donors, in particular of differently hydrated alkali metal silicates, which cause swelling and wetting of dried-on food residues, which cannot be removed from the dishes by the water mechanics alone.
• This layer has a dissolving speed in flowing water of 15 to 40, preferably 28 to 38, grams per hour at 15 ° C.
• the alkali metal silicates, preferably sodium metasilicates, of the melt layer provided for the pre-rinse cycle are used in the anhydrous and therefore most alkaline form and that of nonahydrate, the most easily water-soluble form.
• the mixture can also contain proportions of pentahydrate.
• the composition of the pre-rinse cleaning agent layer consists of 20 to 100, preferably 30 to 80% by weight sodium metasilicate nonahydrate, 0 to 60, preferably 10 to 50% by weight sodium metasilicate pentahydrate and 0 to 60, preferably 10 to 58% by weight to achieve higher alkalinity. anhydrous sodium metasilicate.
• Electrolytes can also be added to the enamel layer provided for the pre-rinse cycle to further improve solubility, but also to optimize costs. Electrolytes are to be understood as alkali salts of inorganic or organic acids such as, for example, pentasodium triphosphate, sodium sulfate, sodium acetate and sodium citrate. Their share in the total weight of the detergent layer provided for the pre-rinse cycle can be 2 to 10, preferably 2 to 5% by weight.
• the layer provided for the pre-rinse cycle can also be in tablet form and contain alkali metal silicate nonahydrate and pentalkalitriphosphate containing 7 to 22.4, preferably 15 to 18% by weight water of crystallization in a ratio of 0: 1 to 1: 0, preferably 0.35: 1 to 1: 1, based on the anhydrous substances.
• the melt layer suitable for the actual cleaning cycle preferably contains a substantial content of sodium metasilicate and anhydrous pentasodium triphosphate and in addition further cleaning-active substances such as an active chlorine compound.
• Their rate of dissolution in flowing water at 15 ° C. is preferably below 25 grams per hour, in particular in the range from 24.5 to 15 grams per hour.
• the amount of the anhydrous pentaalkali metal triphosphate, preferably pentasodium triphosphate, for the melt layer provided for the cleaning cycle is 5 to 50% by weight, preferably 5 to 45% by weight.
• the alkali metal silicates are advantageously used in the melt layer provided for the cleaning cycle in the form of sodium metasilicate nonahydrate, sodium metasilicate hexahydrate and sodium metasilicate pentahydrate.
• the amounts used are 5 to 60, preferably 10 to 50,% by weight, calculated on anhydrous compounds.
• the water-free compound can also be added, which increases the content of cleaning-active substances.
• the optimum ratio of pentasodium triphosphate to sodium metasilicate, in each case anhydrous, calculated for the melt layer for the cleaning cycle, is 2: 1 to 1: 2, preferably 1: 1 to 1: 1.7.
• a tablet-shaped layer which is rapidly soluble for the cleaning cycle and at increasing temperatures can contain alkali metal silicate and pentaalkali metal phosphate in a weight ratio of 2: 1 to 1: 2, preferably 1: 1 to 1.7: 1, and compounds containing active chlorine.
• the alkali metal silicate used in this layer is preferably the anhydrous product with a grain fraction of less than 0.8 mm. However, a mixture of anhydrous metasilicate and its nonahydrate in a weight ratio of at most 1.2: 1 can also be used.
• Inorganic active chlorine carriers such as chlorinated lime, lithium or calcium hypochlorite can also be used. They are in amounts of 0.2 to 4, preferably from 0.5 to 2 wt .-%, based on the active chlorine content, the z. B. to be determined by iodometric titration, and the entire layer used.
• the total water content of the melt block-shaped cleaning agent layer is 11 to 35, preferably 18 to 30% by weight. It is preferably introduced by the crystal water content of the alkaline substances. The calculations of the water content must therefore be based on these compounds.
• the cleaning performance in the pre-rinse cycle can be improved by adding surfactants.
• Surfactants are usually incompatible with active chlorine-releasing compounds. your simultaneous use in a two-layer compactate without impairing the chlorine carrier is possible if both compounds are separated from each other in a different layer.
• the proportion of surfactant in the layer provided for the pre-rinse cycle is 0.5 to 10% by weight, preferably 1 to 5% by weight, based on the pre-rinse cycle layer.
• Suitable surfactant components are the known low-foaming nonionic surfactants, such as the ethoxylation products of long-chain alcohols and alkylphenols, and the free hydroxyl groups of the polyethylene glycol ether residue can be substituted by ether or acetal groups or by polypropylene glycol ether residues to reduce the tendency to foam.
• the block polymers of ethylene oxide with polypropylene oxide are also suitable.
• the tablet-shaped layers for the pre-rinse and the cleaning cycle are preferably 0.5 to 2.5, preferably 1 to 2% by weight calcium hydrogenphosphate dihydrate (to reduce segregation) and 1 to 5, preferably 2 to 3% by weight as tableting aids.
• a further improvement in the solubility of the tablet layers can be achieved, inter alia, by adding other readily water-soluble salts such as. B. sodium chloride can be achieved, but is usually not necessary with the appropriate choice of starting materials.
• Other usual tableting aids such as. B. lubricants to improve the compressibility (z. B. stearates, talc, glycerides, etc.), disintegrants (z. B. cellulose derivatives, attapulgite (Mg-Al-silicate) etc.) and other auxiliaries can be used in principle, they are undesirable from an application technology point of view and also burden the formulation (costs and additional inert fillers).
• These otherwise customary aids can be dispensed with when producing tablet layers according to the present invention.
• the rate of dissolution of the substances for the individual layers of the melt-block-shaped cleaning agents was determined after the raw material melts had solidified in a laboratory apparatus.
• 15 g of the cleaning agent to be tested which was present as a solid, compact mass in the form of a cuboid (approx. 25 ⁇ 95 ⁇ 15 mm), were placed in a 250 ml wash bottle according to DIN 12596 made of borosilicate glass. The wash bottle was then closed with a Drechsel wash bottle insert and secured with a cut holder. Water was passed through the bottle at an average temperature of 15 ° C. corresponding to the pre-rinse cycle at a rate of 20 l / h and after 15 minutes the amount which had dissolved under these conditions was determined by weighing. The dissolving behavior was defined as the dissolving rate in g / h (see Table 1, amounts in% by weight).
• the desired dissolution profile of a multi-layer, in particular two-layer compactate is to be understood as an almost complete dissolution of the 1st layer with a slight detachment of the 2nd layer in the pre-rinse cycle and a quick and complete dissolution of the remaining compactate at the rising water temperatures in the cleaning cycle of all conventional HGSM.
• the tablets were moved up and down in water at 20 ° C. in such a way that they were at the highest point with the base just at the level of the water surface.
• the amount of water was 800 g, the number of strokes was 25 per minute.
• the time required for the disintegration or dissolution of the individual tablets was measured or, for dissolving times of more than 5 minutes, the residues remaining on the sieve were weighed out after 5 to 10 minutes.
• the sodium metasilicate nonahydrate is first heated to about 55 ° C. and, if necessary, dye is added to make it recognizable. Subsequently, sodium metasilicate pentahydrate and / or electrolyte and / or anhydrous sodium metasilicate and / or nonionic surfactant is added, if necessary, with intensive stirring and stirring is continued until the melt and the solid particles distributed therein are essentially homogeneous.
• the melt for the pre-rinse cleaning agent layer preferably also contains at least one of the other compounds specified.
• sodium metasilicate nonahydrate is first heated to about 55 ° C., all other hydrate-containing constituents, in particular sodium metasilicate pentahydrate, then anhydrous pentasodium triphosphate, anhydrous sodium metasilicate and finally the active chlorine-releasing compounds are added and stirred.
• Easily pourable melts preferably have viscosities of approx. 500 to 1,500 mPas, but higher and lower viscosities can also be processed.
• the melts are filled into the intended forms in the quantities to be dosed via a spray nozzle.
• the shapes consist of a z. B. from Polyethylene, polypropylene or polyvinyl chloride manufactured thermoformed part, which also serves as packaging.
• several casting molds can be drawn from film webs in one work process, which can then be filled at the same time using appropriate metering devices.
• the compressibility of raw material mixtures containing almost anhydrous sodium metasilicate to tablet layers depends on the particle size distribution. With a fine grain fraction (smaller than 0.8 mm), good tabletting properties of the raw material mixture are obtained, while dust (smaller than 0.2 mm) and unscreened material (20 to 100% larger than 0.8 mm) lead to mixtures that are difficult to tablettable .
• completely anhydrous metasilicates e.g. manufactured after a sintering or melting process
• the tablets are mechanically stable even after storage.
• hydrothermally produced metasilicate with a residual moisture content of approx. 2% the grain size distribution did not play a decisive role. However, after the tablets had been stored under indoor climate conditions, the surface had weathered. Large tablets then also tend to crack. A residual moisture content of more than 2% in the metasilicate is therefore undesirable.
• Metasilicates in anhydrous form and as nonahydrate and also the anhydrous triphosphate are preferably used in the form of their sodium salts. Their total amount in the mixture to be pressed for the cleaning cycle was 88 to 98, preferably 95 to 97% by weight.
• nonionic surfactant into pre-rinse tablets by using a colored premix of sodium metasilicate nonahydrate and nonionic surfactant without deteriorating their solubility.
• the mixture of the fine-grained, anhydrous metasilicates, the corresponding nonahydrates, the triphosphates, active chlorine carriers and tabletting aids can be pressed under die lubrication, with conventional lubricants being used.
• lubrication is carried out directly through holes in the die, by spraying the lower punch or by means of felt rings soaked in lubricant on the lower punch.
• the raw material mixtures according to the invention with their particularly favorable compressibility properties, however, the lubrication can usually also be dispensed with.
• the pressing conditions must be optimized with a view to setting the desired dissolution profile while at the same time having sufficient tablet hardness.
• the flexural strength can serve as a measure of the tablet hardness (method: compare Ritschel. Die Tablette, Ed. Cantor, 1966, p. 313). Tablets with a flexural strength greater than 12 kp, preferably greater than 15 kp, are sufficiently stable under simulated transport conditions.
• Corresponding tablet hardnesses have been achieved at compression pressures of 500 to 5,000 kp / cm2, preferably 1,000 to 1,500 kp / cm2. Higher pressures reduce the release speed. Soluble Differences in speed can be compensated within limits for different compositions by choosing the pressure.
• the specific weight of the compacts was between 1.2 and 2 g / cm3, preferably between 1.4 and 1.7 g / cm3.
• the compression during the pressing process caused changes in the specific volume, that of 0.8 to 1.8 cm3 / g, preferably 1.0 to 1.4 cm3 / g to 0.5 to 0.8 cm3 / g, preferably 0.6 decreased to 0.7 cm3 / g.
• the shape of the tablet can also influence the dissolving speed via the outer surface exposed to the H20 attack. For stability reasons, cylindrical compacts with a diameter / height ratio of 0.6 to 1.5: 1 were produced.
• the Kompaktate should be manufactured with a total weight of 40 to 60 g each. This corresponds to your preferred application concentration. Lighter compact products can of course also be produced, of which several may then have to be used simultaneously.
• the described compositions can be pressed in a known manner using commercially available eccentric presses or rotary presses.
• the detergent melt is poured into a provided container, preferably deep-drawn parts, which also serve as packaging, poured.
• the tablet for the pre-rinse cycle is then pressed into the still liquid melt mass by hand or by suitable mechanical devices, so that a solid connection between the tablet and the melt block is achieved when the melt solidifies.
• a variant is preferred in which the tablet protrudes from the surface of the melt, so that water access to the tableted portion of the compact is facilitated in the pre-rinse cycle.
• the entire detergent compact can preferably be sealed off in the molded container by means of a peel-off film.
• the compactates can be placed openly in a zone that exposes the compactates to the dissolving power of the tap water flow x, preferably in the cutlery basket of a household dishwasher, even before the pre-rinse cycle begins and the automatically controlled cleaning process is started.
• the invention therefore also relates to the use of the detergent compact for cleaning dishes in automatic household dishwashers, which is characterized in that the compactates are opened in the machine before the pre-rinse cycle begins, for example in a zone which exposes the tablets to the dissolving power of the cold tap water flow by placing it in the cutlery basket, and then initiating the automatically controlled cleaning process.
• the dishes cleaned in this way have better cleaning results for difficult soiling, such as, for example, burnt-on milk or baked oatmeal, than those treated in the conventional manner.
• Formulation of the tablet mixture % By weight 57 pentasodium triphosphate. 18% H20 39 sodium metasilicate nonahydrate 1 C12-C18 fatty alcohol + 5 E0 + 4 P0 0.08 Alizarin Brilliant Pure Blue GLW 2 sodium acetate, anhydrous 1 CaHP04. H20
• the premix of the tablet raw materials was compressed on an eccentric press to give 12.5 g tablets with a diameter of 30 mm and a height of approx. 13 mm.
• sodium metasilicate nonahydrate was first melted in a heated stirred kettle and heated to 57 ° C.
• Sodium metasilicate pentahydrate, pentasodium triphosphate, anhydrous and sodium metasilicate, anhydrous were then incorporated in succession within the shortest possible time with vigorous stirring.
• the melt containing solids was homogenized and heated to approx. 57 ° C.
• the trichloroisocyanuric acid was stirred into the melt.
• 37.5 g of the melt were filled per container shape (deep-drawn parts made of 400 ⁇ PVC film, base area 36 ⁇ 36 mm2, drawing depth 25 mm, free surface 44 ⁇ 44 mm2) using a heated piston metering pump.
• one tablet was pressed so deeply into the still liquid mass that it still protruded about 2 to 4 mm from the surface of the melt.
• a compact obtained in this way was placed in the cutlery basket of a household dishwasher. After the pre-rinse, 36% of the compact was dissolved, the tablet being practically completely removed. The rest of the compactate completely dissolved during the heating of the water that ran into the cleaning cycle.
• a tablet formulation intended for the cleaning cycle (Tables 1, 10 to 12) can be provided with a melt layer which is readily soluble in cold water (Table 2 a), 1 to 6) by pouring over or immersing it.

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• Chemical & Material Sciences (AREA)
• Life Sciences & Earth Sciences (AREA)
• Engineering & Computer Science (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Wood Science & Technology (AREA)
• Organic Chemistry (AREA)
• Inorganic Chemistry (AREA)
• Detergent Compositions (AREA)

Applications Claiming Priority (2)

Publications (2)

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ID=6286455

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Cited By (23)

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• 1985
  • 1985-11-21 DE DE19853541147 patent/DE3541147A1/de not_active Withdrawn
• 1986
  • 1986-11-13 EP EP86115765A patent/EP0224135A3/fr not_active Withdrawn
  • 1986-11-18 CA CA000523272A patent/CA1291918C/fr not_active Expired - Fee Related
  • 1986-11-21 JP JP61279536A patent/JPS62129396A/ja active Pending
• 1989
  • 1989-01-24 US US07/302,067 patent/US4913832A/en not_active Expired - Fee Related

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