EP0791048B1 - Verfahren zur herstellung von wasch- und reinigungsmitteltabletten durch mikrowellen- und heissluftbehandlung - Google Patents
Verfahren zur herstellung von wasch- und reinigungsmitteltabletten durch mikrowellen- und heissluftbehandlung Download PDFInfo
- Publication number
- EP0791048B1 EP0791048B1 EP95937027A EP95937027A EP0791048B1 EP 0791048 B1 EP0791048 B1 EP 0791048B1 EP 95937027 A EP95937027 A EP 95937027A EP 95937027 A EP95937027 A EP 95937027A EP 0791048 B1 EP0791048 B1 EP 0791048B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- hot air
- tablets
- microwave
- minutes
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
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
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0047—Detergents in the form of bars or 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
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S159/00—Concentrating evaporators
- Y10S159/26—Electric field
Definitions
- the invention relates to a method for producing detergent tablets using microwave technology and one Hot air treatment.
- hydrated raw materials are those that contain bound water of crystallization contain or which are able to add water added from the outside bind at least partially as water of crystallization or such substances, that do not form defined hydrates, but are able to form water tie, e.g. Alkali hydroxides.
- microwaves is understood to mean the entire frequency range between 3 and 300,000 MHz, which thus also includes the radio wave range of 3 to 300 MHz in addition to the actual microwave range of above 300 MHz.
- macrosolids can be produced, which, in addition to tablets, also include blocks.
- the premixes are connected to one another at the contact points by local melting / sintering caused by the microwave beams.
- the voids that exist between the individual premix components prior to irradiation with microwaves result in a high porosity of the resulting tablet and thus contribute to improving the dissolving properties of the tablet.
- premix components In order for local sintering of the premix components to be possible, at least some of them must have sintering properties on the surface. For this it is necessary that the premix components themselves or their surface contain enough water so that heating of this water causes the contact points on the premix components to fuse. According to the teaching of the international patent application PCT / EP94 / 01330, at least part of the mixture to be irradiated with microwaves must be in a hydrated form.
- tablettes is therefore not limited to a specific spatial shape; in principle, every conceivable three-dimensional shape possible, depending on which outer shape the powder or granular premixes, e.g. through the container used is imposed.
- the object of the present invention is therefore to find a method at the above Disadvantages do not occur, i.e. with the tablets received that have a high breaking strength and at the same time none Charring.
- the object is achieved in that with during the irradiation process Microwaves a treatment of the premix with hot air at a temperature from 50 ° C to 300 ° C, preferably 100 ° C to 250 ° C, especially 150 ° C to 220 ° C.
- Suitable framework substances are, for example, amorphous silicates such as metasilicates or water glasses, phosphates, alkali carbonates, alkali sulfates, zeolites, but also organic components such as water-containing citrates, for example sodium citrate dihydrate, or water-containing acetates, for example sodium acetate trihydrate.
- Suitable substitutes or partial substitutes for phosphates and zeolites are crystalline, layered sodium silicates of the general formula NaMSi x O 2x + 1 .yH 2 O, where M is sodium or hydrogen, x is a number from 1.9 to 4 and y is a number from 0 to 20 and preferred values for x are 2, 3 or 4.
- Such crystalline layered silicates are described, for example, in European patent application EP-A-0 164 514.
- Preferred crystalline layered silicates are those in which M is sodium and x is 2 or 3.
- both ⁇ and ⁇ -sodium disilicates Na 2 Si 2 O 5 .yH 2 O are preferred.
- Useful organic builder substances are preferred, for example polycarboxylic acids used in the form of their sodium salts, such as citric acid, Adipic acid, succinic acid, glutaric acid, tartaric acid, sugar acids, Aminocarboxylic acids, nitrilotriacetic acid (NTA), provided such use is not objectionable for ecological reasons, as well as mixtures from these.
- Preferred salts are the salts of polycarboxylic acids such as citric acid, Adipic acid, succinic acid, glutaric acid, tartaric acid, sugar acids and mixtures of these.
- Suitable polymeric polycarboxylates are, for example, the sodium salts polyacrylic acid or polymethacrylic acid, for example those with a relative molecular weight of 800 to 150,000 (based on acid).
- Suitable copolymeric polycarboxylates are, in particular, those of acrylic acid with methacrylic acid and acrylic acid or methacrylic acid with maleic acid. Copolymers of acrylic acid with maleic acid have proven particularly suitable proven that 50 to 90 wt .-% acrylic acid and 50 to 10 wt .-% maleic acid contain.
- Their relative molecular mass, based on free acids is generally 5,000 to 200,000, preferably 10,000 to 120,000 and in particular 50,000 to 100,000.
- Organic are also particularly preferred Degradable terpolymers, for example those which are salts of the monomers Acrylic acid and maleic acid as well as vinyl alcohol or vinyl alcohol derivatives (P 43 00 772.4) or the monomers as salts of acrylic acid and Contain 2-alkylallylsulfonic acid and sugar derivatives (DE 42 21 381).
- Suitable builder systems are oxidation products of carboxyl-containing ones Polyglucosans and / or their water-soluble salts as they described for example in the international patent application WO-A-93/08251 be or their production, for example, in the international Patent application WO-A-93/16110 is described.
- polyacetals which by reaction of dialdehydes with polyol carboxylic acids, which have 5 to 7 carbon atoms and have at least 3 hydroxyl groups, for example as in European Patent application EP-A-0 280 223 can be obtained.
- Preferred polyacetals are derived from dialdehydes such as glyoxal, glutaraldehyde, Terephthalaldehyde and mixtures thereof and from polyol carboxylic acids such as gluconic acid and / or glucoheptonic acid.
- the inorganic and / or organic builder substances are preferred in amounts of about 10 to 60% by weight, in particular from 15 to 50 % By weight, used in the tablets.
- Solid acids are used to manufacture acidic detergent tablets such as. Amidosulfonic acid or phosphonic acids are used.
- non-ionic surfactants as described in PCT / EP94 / 01330 are disclosed; nonionic surfactants such as e.g. Fatty alcohol ethoxylates.
- bleach may be used based on oxygen or chlorine, disinfectants e.g. B. quaternary ammonium compounds, foam inhibitors, enzymes, fillers etc. included.
- the duration of the irradiation process is usually between 15 seconds and 90 minutes, preferably between 1 minute and 30 minutes, in particular between 1 minute and 5 minutes.
- hot air treatment can take any length of time, usually however at most 24 hours, preferably at most 60 minutes, especially at most 2 minutes.
- the duration of the hot air treatment can in principle as long as the tablet does not damage the hot air treatment survives; for economic reasons it is up to 30 minutes, preferably up to 10 minutes, especially up to 3 minutes.
- a method is particularly preferred in which the treatment with hot air takes place both during the irradiation process and after the irradiation.
- the duration of the hot air treatment is usually in the period already mentioned above.
- the hot air is generally by a conventional hot air blower with adjustable Air temperature generated.
- the microwave radiation can be carried out, for example, in a microwave oven as described in PCT / EP94 / 01330; the products irradiated in this way can then be subjected to hot air treatment. It is also possible to carry out microwave radiation and hot air treatment in the furnace at the same time.
- the microwave radiation and / or hot air treatment can accordingly - as described - be carried out in batches in a device, for example an oven.
- the microwave irradiation (with simultaneous or subsequent or both simultaneous and subsequent hot air treatment) is preferably carried out in a continuous manner.
- a system is particularly suitable for this purpose in which the premixes to be irradiated are transported on a conveyor belt through a zone irradiated with microwaves.
- hot air is either blown directly into the irradiated zone or into a zone which immediately adjoins the irradiated zone or both into the irradiated zone and into the adjoining zone.
Landscapes
- 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)
- Detergent Compositions (AREA)
Description
Damit überhaupt ein lokales Sintern der Vorgemischbestandteile möglich ist, muß zumindest ein Teil von ihnen Sintereigenschaften an der Oberfläche besitzen. Dazu ist es erforderlich, daß die Vorgemischbestandteile selber oder deren Oberfläche genügend Wasser enthalten, so daß durch Erhitzung dieses Wassers eine Verschmelzung der Kontaktstellen an den Vorgemischbestandteilen erfolgt. Gemäß der Lehre der internationalen Patentanmeldung PCT/EP94/01330 muß zumindest ein Teil der mit Mikrowellen zu bestrahlenden Mischung in hydratisierter Form vorliegen.
Auch die Dauer der Heißluftbehandlung liegt üblicherweise in dem oben bereits erwähnten Zeitraum.
Die Mikrowellenbestrahlung und/oder Heißluftbehandlung kann demnach - wie beschrieben - in einer Vorrichtung, z.B. einem Ofen, chargenweise erfolgen.
Dazu bietet sich insbesondere ein System an, in dem die zu bestrahlenden Vorgemische auf einem Fließband durch eine mit Mikrowellen bestrahlte Zone transportiert werden. Zusätzlich wird entweder direkt in die bestrahlte Zone Heißluft eingeblasen oder aber in eine Zone, die sich der bestrahlten Zone unmittelbar anschließt oder aber sowohl in die bestrahlte Zone als auch in die sich anschließende Zone.
Arbeitsbedingungen: | |
Fließbandgeschwindigkeit | 47 cm pro Minute |
Länge der bestrahlten Zone | 210 cm |
Mikrowellenquelle | 18 Mikrowellenstrahler mit je 1200 Watt Leistung, Wellenlänge 2450 - 2470 MHz |
Abstand von Mikrowelllenquelle zum Fließband | 9 Strahler à 11 cm Abstand 9 Strahler à 4 cm Abstand |
Rezeptur 1 | Amidosulfonsulfonsäure | 96 Gew.-% |
Octanphosphonsäure | 1 Gew.-% | |
C12-18-Fettalkoholethoxylat | 1 Gew.-% | |
Na2SO4 | 1 Gew.-% | |
H2O | 1 Gew.-% | |
Rezeptur 2 | Pentanatriumtriphosphat | 40 Gew.-% |
Natrium-metasilikat | 40 Gew.-% | |
Natrium-metasilikat-Pentahydrat | 10 Gew.-% | |
Natriumcarbonat-Decahydrat | 5 Gew.-% | |
Dimethyldioctylammoniumchlorid | 3 Gew.-% | |
C12-18-Fettalkoholethoxylat | 2 Gew.-% |
Claims (5)
- Verfahren zur Herstellung von Wasch- und Reinigungsmitteltabletten durch Bestrahlung eines Vorgemischs enthalten mindestens eine mindestens teilweise hydratisierte Komponente mit Mikrowellen des Frequenzbereichs 3 bis 300.000 MHz, dadurch gekennzeichnet, daß während des Bestrahlungsvorgangs eine Behandlung mit Heißluft einer Temperatur von 50°C bis 300°C, vorzugsweise 100°C bis 250°C, insbesondere 150 °C bis 200 °C, erfolgt.
- Verfahren zur Herstellung von Wasch- und Reinigungsmitteltabletten durch Bestrahlung eines Vorgemischs mit Mikrowellen, dadurch gekennzeichnet, daß höchstens 24 Stunden, vorzugsweise höchstens 60 Minuten, insbesondere höchstens 2 Minuten, nach Beendigung des Bestrahlungsvorgangs für eine Dauer von bis zu 30 Minuten, vorzugsweise bis zu 10 Minuten, insbesondere bis zu 3 Minuten eine Nachbehandlung mit Heißluft einer Temperatur von 50°C bis 300°C, vorzugsweise 100°C bis 250°C, insbesondere 150°C bis 220°C, erfolgt.
- Verfahren zur Herstellung von Wasch- und Reinigungsmitteltabletten durch Bestrahlung mit Mikrowellen, dadurch gekennzeichnet, daß sowohl eine gleichzeitige Heißluftbehandlung gemäß Anspruch 1, als auch eine sich anschließende Heißluftbehandlung gemäß Anspruch 2 erfolgt.
- Verfahren nach Anspruch 1, 2 oder 3, dadurch gekennzeichnet, daß die Mikrowellenbestrahlung mit gleichzeitiger oder darauffolgender oder sowohl gleichzeitiger als auch darauffolgender Heißluftbehandlung chargenweise erfolgt.
- Verfahren nach Anspruch 1, 2 oder 3, dadurch gekennzeichnet, daß die Mikrowellenbestrahlung mit gleichzeitiger oder darauffolgender oder sowohl gleichzeitiger als auch darauffolgender Heißluftbehandlung kontinuierlich erfolgt.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE4439679A DE4439679A1 (de) | 1994-11-07 | 1994-11-07 | Verfahren zur Herstellung von Wasch- und Reinigungsmitteltabletten durch Mikrowellen- und Heißluftbehandlung |
DE4439679 | 1994-11-07 | ||
PCT/EP1995/004242 WO1996014391A1 (de) | 1994-11-07 | 1995-10-30 | Verfahren zur herstellung von wasch- und reinigungsmitteltabletten durch mikrowellen- und heissluftbehandlung |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0791048A1 EP0791048A1 (de) | 1997-08-27 |
EP0791048B1 true EP0791048B1 (de) | 1999-06-02 |
Family
ID=6532650
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP95937027A Expired - Lifetime EP0791048B1 (de) | 1994-11-07 | 1995-10-30 | Verfahren zur herstellung von wasch- und reinigungsmitteltabletten durch mikrowellen- und heissluftbehandlung |
Country Status (11)
Country | Link |
---|---|
US (1) | US5914309A (de) |
EP (1) | EP0791048B1 (de) |
AT (1) | ATE180827T1 (de) |
DE (2) | DE4439679A1 (de) |
DK (1) | DK0791048T3 (de) |
ES (1) | ES2135101T3 (de) |
FI (1) | FI971932A0 (de) |
GR (1) | GR3030495T3 (de) |
NO (1) | NO971303D0 (de) |
NZ (1) | NZ295667A (de) |
WO (1) | WO1996014391A1 (de) |
Families Citing this family (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE69914582T2 (de) * | 1998-02-10 | 2004-08-05 | Unilever N.V. | Waschmittel in tablettenform |
GB9807992D0 (en) * | 1998-04-15 | 1998-06-17 | Unilever Plc | Water softening and detergent compositions |
GB9822090D0 (en) * | 1998-10-09 | 1998-12-02 | Unilever Plc | Detergent Compositions |
DE19948668A1 (de) * | 1999-10-08 | 2001-04-19 | Cognis Deutschland Gmbh | Waschmitteltabletten |
DE10010760A1 (de) * | 2000-03-04 | 2001-09-20 | Henkel Kgaa | Mehrphasige Wasch- und Reinigungsmittelformkörper mit nicht-gepreßten Anteilen |
DE10125441A1 (de) * | 2001-05-25 | 2002-12-05 | Henkel Kgaa | Verfahren und benötigte Zusätze zur Erhöhung der Stabilität von Tabletten |
DE10254314B4 (de) * | 2002-11-21 | 2004-10-14 | Henkel Kgaa | Verfahren zur Herstellung befüllter Wasch- und Reinigungsmittelformkörper II |
US8039531B2 (en) * | 2003-03-14 | 2011-10-18 | Eastman Chemical Company | Low molecular weight cellulose mixed esters and their use as low viscosity binders and modifiers in coating compositions |
US7585905B2 (en) * | 2003-03-14 | 2009-09-08 | Eastman Chemical Company | Low molecular weight cellulose mixed esters and their use as low viscosity binders and modifiers in coating compositions |
US8124676B2 (en) * | 2003-03-14 | 2012-02-28 | Eastman Chemical Company | Basecoat coating compositions comprising low molecular weight cellulose mixed esters |
US8461234B2 (en) * | 2003-03-14 | 2013-06-11 | Eastman Chemical Company | Refinish coating compositions comprising low molecular weight cellulose mixed esters |
US20070282038A1 (en) * | 2006-06-05 | 2007-12-06 | Deepanjan Bhattacharya | Methods for improving the anti-sag, leveling, and gloss of coating compositions comprising low molecular weight cellulose mixed esters |
US20080085953A1 (en) * | 2006-06-05 | 2008-04-10 | Deepanjan Bhattacharya | Coating compositions comprising low molecular weight cellulose mixed esters and their use to improve anti-sag, leveling, and 20 degree gloss |
SMP201200046B1 (it) * | 2012-10-24 | 2015-07-09 | Caffemotive Srl | Un metodo per la produzione di una compressa di unprodotto macinato in polvere per l'estrazione di bevande nonchè compressa ottenibile con tale metodo |
Family Cites Families (18)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
NL278464A (de) * | 1961-05-15 | |||
JPS52587B2 (de) * | 1972-04-11 | 1977-01-08 | ||
DE2327956A1 (de) * | 1973-06-01 | 1974-12-19 | Henkel & Cie Gmbh | Verfahren zur herstellung von wasserloesliche hydratisierte salze enthaltenden granulaten, insbesondere wasch- und reinigungsmittelgranulaten |
US4405850A (en) * | 1978-10-06 | 1983-09-20 | Raytheon Company | Combination microwave heating apparatus |
US4584281A (en) * | 1981-09-18 | 1986-04-22 | The Clorox Company | Controlled delivery of immiscible materials into an aqueous system |
DE3413571A1 (de) * | 1984-04-11 | 1985-10-24 | Hoechst Ag, 6230 Frankfurt | Verwendung von kristallinen schichtfoermigen natriumsilikaten zur wasserenthaertung und verfahren zur wasserenthaertung |
US4885108A (en) * | 1986-08-12 | 1989-12-05 | Colgate-Palmolive Company | Method of shaping of soap bar |
DE3706036A1 (de) * | 1987-02-25 | 1988-09-08 | Basf Ag | Polyacetale, verfahren zu deren herstellung aus dialdehyden und polyolcarbonsaeuren und verwendung der polyacetale |
DE4010533A1 (de) * | 1990-04-02 | 1991-10-10 | Henkel Kgaa | Tablettierte wasch- und/oder reinigungsmittel fuer haushalt und gewerbe und verfahren zu ihrer herstellung |
US5108646A (en) * | 1990-10-26 | 1992-04-28 | The Procter & Gamble Company | Process for agglomerating aluminosilicate or layered silicate detergent builders |
BE1004876A5 (fr) * | 1991-05-27 | 1993-02-16 | Serstevens Albert T | Perfectionnement pour l'obtention de poudres a lessiver par micro-ondes. |
DE4134914A1 (de) * | 1991-10-23 | 1993-04-29 | Henkel Kgaa | Wasch- und reinigungsmittel mit ausgewaehlten builder-systemen |
DE4221381C1 (de) * | 1992-07-02 | 1994-02-10 | Stockhausen Chem Fab Gmbh | Pfropf-Copolymerisate von ungesättigten Monomeren und Zuckern, Verfahren zu ihrer Herstellung und ihre Verwendung |
DE4203923A1 (de) * | 1992-02-11 | 1993-08-12 | Henkel Kgaa | Verfahren zur herstellung von polycarboxylaten auf polysaccharid-basis |
DE4300772C2 (de) * | 1993-01-14 | 1997-03-27 | Stockhausen Chem Fab Gmbh | Wasserlösliche, biologisch abbaubare Copolymere auf Basis von ungesättigten Mono- und Dicarbonsäuren, Verfahren zu ihrer Herstellung und ihre Verwendung |
ATE207109T1 (de) * | 1993-05-05 | 2001-11-15 | Henkel Ecolab Gmbh & Co Ohg | Verfahren zum verfestigen von teilchenfoermigen feststoffen und reinigungsprodukte daraus |
DE4429550A1 (de) * | 1994-08-19 | 1996-02-22 | Henkel Kgaa | Verfahren zur Herstellung von Wasch- oder Reinigungsmitteltabletten |
DE19601840A1 (de) * | 1996-01-19 | 1997-07-24 | Henkel Kgaa | Verfahren zur Herstellung von Wasch- oder Reinigungsmittelformkörpern |
-
1994
- 1994-11-07 DE DE4439679A patent/DE4439679A1/de not_active Withdrawn
-
1995
- 1995-10-30 WO PCT/EP1995/004242 patent/WO1996014391A1/de active IP Right Grant
- 1995-10-30 AT AT95937027T patent/ATE180827T1/de not_active IP Right Cessation
- 1995-10-30 US US08/836,623 patent/US5914309A/en not_active Expired - Lifetime
- 1995-10-30 DE DE59506121T patent/DE59506121D1/de not_active Expired - Fee Related
- 1995-10-30 DK DK95937027T patent/DK0791048T3/da active
- 1995-10-30 NZ NZ295667A patent/NZ295667A/xx unknown
- 1995-10-30 ES ES95937027T patent/ES2135101T3/es not_active Expired - Lifetime
- 1995-10-30 EP EP95937027A patent/EP0791048B1/de not_active Expired - Lifetime
-
1997
- 1997-03-20 NO NO971303A patent/NO971303D0/no not_active Application Discontinuation
- 1997-05-06 FI FI971932A patent/FI971932A0/fi unknown
-
1999
- 1999-06-10 GR GR990401570T patent/GR3030495T3/el unknown
Also Published As
Publication number | Publication date |
---|---|
FI971932A (fi) | 1997-05-06 |
WO1996014391A1 (de) | 1996-05-17 |
FI971932A0 (fi) | 1997-05-06 |
NO971303L (no) | 1997-03-20 |
EP0791048A1 (de) | 1997-08-27 |
NZ295667A (en) | 1998-10-28 |
DE59506121D1 (de) | 1999-07-08 |
ATE180827T1 (de) | 1999-06-15 |
DK0791048T3 (da) | 1999-12-13 |
GR3030495T3 (en) | 1999-10-29 |
NO971303D0 (no) | 1997-03-20 |
ES2135101T3 (es) | 1999-10-16 |
DE4439679A1 (de) | 1996-05-09 |
US5914309A (en) | 1999-06-22 |
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