EP0167916A2 - Procédé de préparation d'un adjuvant de détergent non ionique séché par pulvérisation - Google Patents

Procédé de préparation d'un adjuvant de détergent non ionique séché par pulvérisation Download PDF

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Publication number
EP0167916A2
EP0167916A2 EP85107820A EP85107820A EP0167916A2 EP 0167916 A2 EP0167916 A2 EP 0167916A2 EP 85107820 A EP85107820 A EP 85107820A EP 85107820 A EP85107820 A EP 85107820A EP 0167916 A2 EP0167916 A2 EP 0167916A2
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EP
European Patent Office
Prior art keywords
weight
component
spray
water
parts
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.)
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Application number
EP85107820A
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German (de)
English (en)
Other versions
EP0167916A3 (fr
Inventor
Wolfgang Dr. Seiter
Ingo Wegener
Herbert Dr. Reuter
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
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Application filed by Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Publication of EP0167916A2 publication Critical patent/EP0167916A2/fr
Publication of EP0167916A3 publication Critical patent/EP0167916A3/fr
Withdrawn legal-status Critical Current

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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
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/02—Preparation in the form of powder by spray drying
    • 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
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66—Non-ionic compounds
    • C11D1/72—Ethers of polyoxyalkylene glycols
    • 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
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246—Silicates, e.g. diatomaceous earth
    • C11D3/128—Aluminium silicates, e.g. zeolites

Definitions

  • Washing aids are understood to mean products which on their own are not wholesome, i.e. H. are able to meet all the requirements for a heavy-duty detergent, but can be added to pre-made detergents as additives or used as a detergent booster in conventional washing processes in order to better solve special cleaning tasks.
  • Non-ionic surfactants have proven their worth as detergent boosters, especially for stubborn stains.
  • detergents usually already contain fractions of nonionic surfactants in the order of 3 to 20% by weight. However, it is a rule in professional circles that specifically light, ie a bulk density of less than 600 g / l, detergent with a content of more than 8 to 10% by weight of such mostly liquid to semisolid, more or less tendency to stick non-ionic surfactants can no longer be produced without problems by spray drying aqueous concentrates (slurries).
  • DE-AS 17 92 434 discloses a process for the production of granular detergents containing 5 to 20% of nonionic surfactants by spray drying an aqueous batch.
  • carrier material such as sulfates, silicates and phosphates
  • powders with a bulk density of 300 to 800 g / l and a nonionic surfactant content of up to 25% by weight should be able to be produced.
  • post-treatment prowdering
  • an adsorbent such as silica airgel or carboxymethyl cellulose is required.
  • Such a 3-stage manufacturing process is comparatively complex.
  • Granular detergents with a bulk density of at least 500 g / l which consist of essentially spherical particles of a certain grain size and are said to be able to absorb up to 30% by weight of nonionic surfactants, are also known from German Offenlegungsschrift 27 42 683 (US 4,269,722 ) known. In these cases too, a carrier grain with increased absorbency must first be produced by a special spraying method and then treated in a mixer with the nonionic surfactant. These products are also high in phosphate and comparatively complex due to the multi-stage manufacturing process.
  • Suitable nonionic surfactants are ethoxylated alcohols having 12 to 24, preferably 14 to 18 carbon atoms and an average of 3 to 20, preferably 4 to 16, glycol ether groups.
  • the hydrocarbon residues can be saturated or monounsaturated, linear or also methyl-branched in the 2-position (oxo residue) and can be derived, for example, from naturally occurring or hydrogenated fat residues and / or synthetic residues.
  • Ethoxylates derived from cetyl, stearyl and oleyl alcohol and mixtures thereof have proven to be particularly suitable.
  • EO ethylene oxide groups
  • tallow fatty alcohol with an average of 10 to 18 EO tallow fatty alcohol with an average of 10 to 18 EO
  • oleyl alcohol with an average of 6 to 12 EO as well as their mixtures.
  • Such mixtures of two and more surfactants with different EO content, in which the proportion of higher ethoxylated alcohols predominates have proven to be particularly advantageous, since the tendency to smoke formation in the exhaust air (so-called pluming) is particularly low and the washing action against mineral ones and fatty soiling is particularly pronounced.
  • the cited ethoxylated alcohols can be replaced in whole or in part by ethoxylated alkylphenols having 8 to 12 carbon atoms in the alkyl group and 5 to 12 EO groups, but the ethoxylated alcohols are preferably used.
  • the zeolite NaA can be used in particular, also the zeolite NaX and mixtures of NaA and NaX.
  • the agents can be phosphate-free.
  • sodium tripolyphosphate (component D) can be used in proportions of not more than 25% by weight, preferably not more than 20% by weight and in particular not more than 17% by weight. each based on anhydrous substance, are incorporated into the slurry.
  • This additive improves the pourability of the spray powder and its dissolution rate in cold water within certain limits. Since the detergents produced according to the invention are not single-use detergents, but rather are intended as a cleaning-enhancing additive to detergents, the proportion of phosphate is reduced even further in practical use, in particular if a phosphate-free preparation is used as a further detergent component.
  • the content of soap and synthetic anionic surfactants should be less than 3%, preferably not more than 2%.
  • the soap content can be 0.1 to 2% by weight.
  • Higher levels of synthetic anionic surfactants should should not be used, as it has been shown that they lead to a decrease in the pourability.
  • the slurry is added in amounts of 0.1 to 3, in particular 0.3 to 2% by weight, based on anhydrous constituents, of hydroxyalkane polyphosphonic acids of the following formulas in which R is an alkyl radical and R 'is an alkenyl radical having 1 to 4 carbon atoms.
  • R is an alkyl radical and R 'is an alkenyl radical having 1 to 4 carbon atoms.
  • the sodium salt of 1-flydroxyethane-1,1-diphosphonic acid is preferably used.
  • the phosphonic acids counteract thermal decomposition of the nonionic surfactants during the spraying process and reduce the tendency to smoke in the exhaust air as well as the yellowing and browning of the spray powder in the event of caking on the inside of the tower. They also increase the dissolution rate of the powder in cold water.
  • up to 2% by weight, based on anhydrous constituents, of sodium hydroxide in the form of sodium hydroxide solution are additionally added to the aqueous concentrate, which improves the processability of the slurry and the solubility of the spray product in cold water.
  • Fractions of 0.5 to 1.5% by weight of sodium hydroxide have proven to be particularly expedient.
  • a more alkaline sodium silicate (component B) for example the composition Na - 0: Si0 2 as 1: 2, the proportion of sodium hydroxide can be reduced or an addition can be dispensed with without disadvantage.
  • the concentration of the slurry is adjusted so that 50 to 65 parts by weight, preferably 55 to 63 parts by weight of anhydrous constituents account for 50 to 35 parts by weight, preferably 45 to 37 parts by weight of water.
  • the spray drying is carried out in such a way that the dried product contains 9 to 16% by weight, preferably 10 to 15% by weight, of water which can be removed by drying (under atmospheric pressure) at 130.degree.
  • the slurry has a temperature of 60 to 70 ° C., preferably 62 to 68 ° C., in the interest of easy processability, especially when the specified small amounts of soap are also used.
  • the spraying is carried out by means of conventional nozzles, which are generally constructed as swirl nozzles, under a pressure of 35 to 100, preferably 40 to 65 bar.
  • the nozzle opening usually has a diameter of 3 to 5 mm.
  • the dry gas directed towards the sprayed material has an inlet temperature of 160 to 240 ° C, preferably 170 ° C to 220 ° C, this temperature being measured in the so-called ring channel, ie in the inlet area immediately before the lower tower inlets.
  • the outlet temperature of the dry gas is 80 to 95 ° C. Higher inlet temperatures lead to the formation of caking on the tower walls and browning of the baked powder components. Higher outlet temperatures favor undesirable smoke formation in the exhaust air.
  • the ingredients were mixed into an aqueous slurry with a total water content of 57% by weight.
  • the tripolyphosphate was 92% in modification II.
  • the zeolite was used as a stable, aqueous slurry (master-batch) with a water content of 52.1% by weight, the sodium hydroxide as 50% sodium hydroxide solution.
  • the degree of decomposition manifests itself in the different height of a peak, the height of which is given below in cm below the base value.
  • the degree of smoke formation is given in scale parts of the nephelometer, with increasing smoke formation being characterized by larger numbers.
  • the spray powders had a uniform grain spectrum.
  • the average grain size was 0.8 mm.
  • the proportion above 1.6 mm was in the range from 0.5 to 1% by weight, the proportion of fine parts with a grain size below 0.1 mm below 0.5% by weight. In comparative experiment C, however, it was 0.9% by weight.
  • the bulk density of the compositions was between 450 g / 1 and 500 g / 1.
  • packages made of cardboard are evenly filled with the product up to the standard filling level, closed with a lid that can be put on, and compressed in a machine-driven vibrator under defined conditions by directional impacts, which results in a reproducible compression of the contents.
  • the package is opened and fastened in a device that allows it to be poured out at defined tilting angles.
  • the packages can be shaken by means of a motorized impact device.
  • the amount of powder flowing out is collected in a measuring cylinder.
  • Assign ratings with the specified degrees of angle indicating the position of the package:
  • the consumer registers the grades 1 to 3 as very good to good, the grade 4 as satisfactory and the grades 5 and 6 as poor or unsatisfactory.
  • Remnants of substance remaining in the beaker are transferred onto the sieve using as little water as possible.
  • the sieve is weighed in air after a drying time of 24 hours.
  • Grades from 1 to 6 are given for the degree of residue formation, with grade 4 meaning sufficient solubility in practice, ie it comes no residue formation on the washed, unwashed laundry.
  • the grade 6 means that in practice there can be recognizable deposits on the unwashed laundry under cold washing conditions.
  • Table II As in Table I, the examples falling within the scope of the invention are identified by numbers, the comparative examples by letters.

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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)
EP85107820A 1984-07-02 1985-06-24 Procédé de préparation d'un adjuvant de détergent non ionique séché par pulvérisation Withdrawn EP0167916A3 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3424299A DE3424299A1 (de) 1984-07-02 1984-07-02 Verfahren zur herstellung eines spruehgetrockneten nichtionischen waschhilfsmittels
DE3424299 1984-07-02

Publications (2)

Publication Number Publication Date
EP0167916A2 true EP0167916A2 (fr) 1986-01-15
EP0167916A3 EP0167916A3 (fr) 1987-07-01

Family

ID=6239629

Family Applications (1)

Application Number Title Priority Date Filing Date
EP85107820A Withdrawn EP0167916A3 (fr) 1984-07-02 1985-06-24 Procédé de préparation d'un adjuvant de détergent non ionique séché par pulvérisation

Country Status (3)

Country Link
US (1) US4661281A (fr)
EP (1) EP0167916A3 (fr)
DE (1) DE3424299A1 (fr)

Families Citing this family (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3545947A1 (de) * 1985-12-23 1987-07-02 Henkel Kgaa Phosphatfreies, granulares waschmittel
DE3630533A1 (de) * 1986-09-08 1988-03-10 Henkel Kgaa Neue tensidgemische und ihre verwendung
DE3842007A1 (de) * 1988-12-14 1990-06-21 Henkel Kgaa Fluessiges bis pastoeses, bleichmittelhaltiges waschmittel
ATE131862T1 (de) * 1991-08-13 1996-01-15 Procter & Gamble Verfahren zur herstellung eines granularen maschinengeschirrspuelmittels
US5219495A (en) * 1991-12-16 1993-06-15 Lever Brothers Company, Division Of Conopco, Inc. Detergent compositions containing mobile liquid active systems
US5565422A (en) * 1995-06-23 1996-10-15 The Procter & Gamble Company Process for preparing a free-flowing particulate detergent composition having improved solubility
DE19936726A1 (de) * 1999-08-06 2001-02-08 Henkel Kgaa Verfahren zur Herstellung cobuilder-haltiger Zubereitungen
DE10063762A1 (de) * 2000-12-21 2002-06-27 Cognis Deutschland Gmbh Nichtionische Tenside
CN104997634A (zh) 2010-04-09 2015-10-28 帕西拉制药有限公司 用于配制大直径合成膜囊泡的方法
US8939388B1 (en) 2010-09-27 2015-01-27 ZoomEssence, Inc. Methods and apparatus for low heat spray drying
US9332776B1 (en) 2010-09-27 2016-05-10 ZoomEssence, Inc. Methods and apparatus for low heat spray drying
US10486173B2 (en) 2017-08-04 2019-11-26 ZoomEssence, Inc. Ultrahigh efficiency spray drying apparatus and process
US10155234B1 (en) 2017-08-04 2018-12-18 ZoomEssence, Inc. Ultrahigh efficiency spray drying apparatus and process
JP7177136B2 (ja) 2017-08-04 2022-11-22 ズーメッセンス，インコーポレイテッド 超高効率噴霧乾燥装置及びプロセス
US9861945B1 (en) 2017-08-04 2018-01-09 ZoomEssence, Inc. Ultrahigh efficiency spray drying apparatus and process
US9993787B1 (en) 2017-08-04 2018-06-12 ZoomEssence, Inc. Ultrahigh efficiency spray drying apparatus and process
US10569244B2 (en) 2018-04-28 2020-02-25 ZoomEssence, Inc. Low temperature spray drying of carrier-free compositions

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2340984A1 (fr) * 1976-02-10 1977-09-09 Unilever Nv Procede pour preparer des compositions detergentes
DE2724349A1 (de) * 1977-05-28 1978-12-07 Henkel Kgaa Verfahren zur herstellung spruehgetrockneter, nichtionische tenside enthaltender waschmittel
EP0036162A1 (fr) * 1980-03-17 1981-09-23 Henkel Kommanditgesellschaft auf Aktien Produit de lavage à faible teneur en phosphates et à mousse régulée
EP0061226A1 (fr) * 1981-03-23 1982-09-29 THE PROCTER & GAMBLE COMPANY Compositions détergentes séchées par atomisation
EP0120492A2 (fr) * 1983-03-25 1984-10-03 Henkel Kommanditgesellschaft auf Aktien Composante granuleuse de détergent, à écoulement libre et procédé pour sa préparation

Family Cites Families (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2550691A (en) * 1951-05-01 Nongorrosive detergent
DE1098132B (de) * 1959-01-14 1961-01-26 Budenheim Rud A Oetker Chemie Verfahren zur Herstellung von Wasch-, Reinigungs-, Spuel- und Entfettungsmitteln in Plverform
NO121968C (fr) * 1966-06-23 1977-06-13 Mo Och Domsjoe Ab
GB1232009A (fr) * 1967-09-04 1971-05-19
GB1371101A (en) * 1971-02-03 1974-10-23 Unilever Ltd Production of detergent compositions
US3838072A (en) * 1971-03-15 1974-09-24 Colgate Palmolive Co Manufacture of free flowing particulate detergent containing nonionic surface active compound
US3886098A (en) * 1971-03-15 1975-05-27 Colgate Palmolive Co Manufacture of free flowing particulate detergent composition containing nonionic detergent
US3849327A (en) * 1971-11-30 1974-11-19 Colgate Palmolive Co Manufacture of free-flowing particulate heavy duty synthetic detergent composition containing nonionic detergent and anti-redeposition agent
US3926827A (en) * 1973-03-29 1975-12-16 Colgate Palmolive Co Method for making detergent compositions
DE2418294B2 (de) * 1974-04-16 1976-11-04 Henkel & Cie GmbH, 4000 Düsseldorf Pulverfoermiges bis koerniges, nichtionische waschaktivsubstanzen enthaltendes waschmittel
DE2431529C2 (de) * 1974-07-01 1982-11-18 Henkel KGaA, 4000 Düsseldorf Verfahren zur Herstellung sprühgetrockneter, nichtionische Tenside enthaltender Waschmittel
US4269722A (en) * 1976-09-29 1981-05-26 Colgate-Palmolive Company Bottled particulate detergent
DE2820554A1 (de) * 1978-05-11 1979-11-22 Hoechst Ag Wasch- und reinigungsmittel
DE2837504C2 (de) * 1978-08-28 1983-07-07 Henkel KGaA, 4000 Düsseldorf Verfahren zur Herstellung eines schüttfähigen, nichtionische Tenside enthaltenden Wasch- und Reinigungsmittelgranulates
US4216125A (en) * 1978-12-07 1980-08-05 Pq Corporation Detergent compositions with silane-zeolite silicate builder

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2340984A1 (fr) * 1976-02-10 1977-09-09 Unilever Nv Procede pour preparer des compositions detergentes
DE2724349A1 (de) * 1977-05-28 1978-12-07 Henkel Kgaa Verfahren zur herstellung spruehgetrockneter, nichtionische tenside enthaltender waschmittel
EP0036162A1 (fr) * 1980-03-17 1981-09-23 Henkel Kommanditgesellschaft auf Aktien Produit de lavage à faible teneur en phosphates et à mousse régulée
EP0061226A1 (fr) * 1981-03-23 1982-09-29 THE PROCTER & GAMBLE COMPANY Compositions détergentes séchées par atomisation
EP0120492A2 (fr) * 1983-03-25 1984-10-03 Henkel Kommanditgesellschaft auf Aktien Composante granuleuse de détergent, à écoulement libre et procédé pour sa préparation

Also Published As

Publication number Publication date
EP0167916A3 (fr) 1987-07-01
DE3424299A1 (de) 1986-01-09
US4661281A (en) 1987-04-28

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