US3562165A - Process for preparing a dry compacted detergent composition - Google Patents

Process for preparing a dry compacted detergent composition Download PDF

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Publication number
US3562165A
US3562165A US625411A US3562165DA US3562165A US 3562165 A US3562165 A US 3562165A US 625411 A US625411 A US 625411A US 3562165D A US3562165D A US 3562165DA US 3562165 A US3562165 A US 3562165A
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Prior art keywords
powder
sodium
compacting
powders
mixture
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US625411A
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English (en)
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Renato Altieri
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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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/395—Bleaching agents
    • C11D3/3953—Inorganic bleaching agents
    • 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
    • C11D17/0069—Laundry bars
    • 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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/39—Organic or inorganic per-compounds
    • 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
    • C11D3/395—Bleaching agents
    • C11D3/3955—Organic bleaching agents
    • 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
    • C11D3/395—Bleaching agents
    • C11D3/3958—Bleaching agents combined with phosphates

Definitions

  • a soap-like compact detergent consisting of a mixture of dry-compacted powder components is produced by mixing the components in the dry state, milling the mixture and compacting the resulting powder in dies with a minimum pressure of about 30 kg./cm.
  • the present invention relates to a compact product based on detergent powder, said product having the shape and compactness of a common soap to be used in fact like a common soap, but which is obtained by a new process for this kind of product.
  • pieces of hard synthetic detergent presently on the market are obtained by the conventional soap making process, consisting essentially of mixing the various components with water, drawing, refining the paste, drawing again, cutting and molding.
  • the product shows in fact, when used, a non smooth and non soft surface. Under the solvent action of the water, when the product is used, there will develop a surface showing a certain sandy aspect or roughness which is very unpleasant and which, if the soap is used as a washing soap can amount to such a degree as to be harmful to the washed fabric, due to abrasive action. Furthermore said manufactured products are not very resistent to elevated room temperatures, tend to become soft and to exude moisture.
  • the dry process also shows a large flexibility of formulation due to the almost total absence of free water in the composition of the product. If the manufactured product is to be used as a washing soap, solid bleaching agents, such as sodium perborate and/or ammonia base compounds and/ or chlorine base compounds can be added to the formulation without affecting the compound itself.
  • solid bleaching agents such as sodium perborate and/or ammonia base compounds and/ or chlorine base compounds
  • the components of the formulation are dry mixed in a powder mixing apparatus of any kind. It is fundamentally important to the effect of the subsequent operations that the free humidity in the mixture of the powders be as low as possible, mainly in order not to affect the good fluency of the powders.
  • the amount of total humidity can also be very high, but said water must be present as crystallization water of one or more components of the formula and not as free water.
  • the mixture will then be ground in a powder mill.
  • the grain size of the powders after milling can range from an impalpable powder to a coarse powder, and said feature has a remarkable importance on the effects of the quality of the product.
  • the roughness of the piece when used depends on the fineness of the ground powder, the formula of the product and upon the pressure exerted when the components are compacted.
  • certain possible components of the formula can cause a roughness in the use of the finished product if they are not ground to an impalpable powder, while other possible components of the formula can remain in a relatively coarse form, without thereby affecting the softness of the feel when the t piece is used.
  • the milling operation of the various ingredients can be carried out before the mixing operation, either individually for each component of the formula or for groups of components.
  • the mixed and ground powders in the desired proportions are then sent directly to a compacting operation without passing through any other intermediate working stage. It has been in fact found that detergent powders having determined compositions if-adequately compressed under pressures of at least 30 kg./ square cm., with particular contrivances in the equipments required for compacting, and provided that said powders are ground at a fineness adequate to the particular formulation which has to be compacted, give products which can be used like common soap, wearing out regularly without foliating or crushing, and being stable through the entire time of use without undergoing degradation even in the most unfavorable ambient conditions.
  • the compacting machine used in this process be of any particular kind. Either a die and punch reciprocating machine (for instance of the kind used for compressing thermosetting resins) or a rotary machine (for instance of the kind used for compacting medicinal products) or a compounded rotary-reciprocating machine can be successfully used. What is essential for the process is a group of technical contrivances and equipment as hereinafter described.
  • the supply of the powder to the die should be carried out 'by vibrating the powders in order to prevent the latter from having a variable apparent density depending on the aeration of said powders, the level of the powder in the feeding hopper, and for preventing bridges from being formed in the dosing device.
  • the above has a particular importance due to the high amount of powder which must be fed into the die.
  • An example of a suitable kind of supply of the powders consist in a constant level hopper fed by a rotary valve controlled by an electric motor.
  • the terminal portion of said hopper has a quadrangular shaped section and is connected by means of a flexible hose to guides on which glides a two compartment drawer having an equal volume and a quadrangular section approximately equal to that of the feeding hopper.
  • Said compartments have hinged movable bottoms, the opening or closing movements of which are controlled by an electromagnet.
  • the top cross sectional area is in immediate contact with the drawer and has such an area as to allow the discharge of the powder into the little hopper, whatever the position of the drawer.
  • the little hopper feeds directly the die into which the powder will be compressed.
  • pre-compacting operation Another essentially important point for the successful issue of the operations is the pre-compacting operation. It is necessary to expel from the powder the maximum possible amount of air before the final compacting, in order to avoid any included air from remaining in the piece when large amounts of powder are compressed at high speed, said air being very harmful since it will cause a great weakening of the product, rendering it brittle and friable instead of hard and compact. Further, without adequate pre-compacting it will be very difficult to obtain high manufacturing capacities as the punch of the press would have to effect too long a stroke and consequently the time required for this operation would be high.
  • the pre-compression can very simply consist of a change of the stroke speed of the punches within the die; in case of rotary presses, in a gradual and relatively slow nearing of the upper punches to the lower punches; in case of compounded system press, the pre-compression can be obtained by one or both of the aforesaid systems.
  • the compacting operation is carried out in the die (which must be slightly conical in order to allow the expulsion of the finished product) into which the powder has been introduced and precompressed.
  • Two punches both movable or either movable operate the actual compacting and give the shape to the manufactured product.
  • the pressure can be supplied by mechanical (eccentric presses, toggle presses, etc.) or by pneumatic or hydrostatic means (oleodynamic or hydrodynamic presses).
  • the manufactured piece can be expelled upward or downward of the die, and the various mechanical systems for embodying said operations are well known.
  • the lubrification operation has to be carried out and this operation can be embodied, either by particular kinds of lubricant powders (for instance talcum, kaolin, starch, silicic acids etc.) which create a very thin film on the surface contacting the detergent powders, or by suitable lubricants (oils, silicone emulsions, water, kerosene, other petroleum derivatives, etc.).
  • lubricant powders for instance talcum, kaolin, starch, silicic acids etc.
  • suitable lubricants oil, silicone emulsions, water, kerosene, other petroleum derivatives, etc.
  • the lubrication can be effected simultaneously with the brushing operation, coupling in the mechanical brushing devices the lubricating devices.
  • the composition of a compact detergent of the type described in the first part of the present invention is very similar to that of the common sprayed detergents.
  • sodium aryl-alkyl sulphonates having variable lengths of chain of the carbon atoms, complexed sodium phosphates such as sodium tii-poly-phosphate or pyro-phosphate, optical coloring agents, carboxymethyl cellulose, sodium carbonate, sodium sulphate, ammonium bicarbonate, waterglass, sodium metasilicate, starch etc.
  • the amount of waterglass (with the aforesaid characteristics) necessary to obtain a product of good quality varies according to the formulation, from 0.5% to 35.0%.
  • the required waterglass can otherwise already exist in the sodium aryl-alkyl-sulphonate (or other sulphonate or sulphate) previously mixed in paste form with the solution of waterglass having the aforesaid features, and then dried.
  • ammonium bicarbonate when contacted with water, inhighly alkaline media, forms ammonia, which, as is known, has a bleaching power; that the sodium perborate, in contact with water, releases active oxygen, having a bleaching and cleaning power; that the chlorinated substances, such as calcium and lithium hypochlorite, the di-chloro and tri-chloro iso cyanuric acids, or also mixed or not, their alkaline and/or alkaline earth metal salts, when contacting water, release active chlorine having cleaning and bleaching power.
  • the chlorinated substances such as calcium and lithium hypochlorite, the di-chloro and tri-chloro iso cyanuric acids, or also mixed or not, their alkaline and/or alkaline earth metal salts, when contacting water, release active chlorine having cleaning and bleaching power.
  • Said materials cannot be used in the normal sprayed detergents or in the compact detergents manufactured by the conventional processes, because the development of ammonia and/or of oxygen and/or of chlorine during the manufacturing process would occur due to the presence of water.
  • said ingredients can be used without risk of decomposition during the manufacturing process or during the storage.
  • the decomposition occurs, on the contrary, when the compact detergents are used, i.e. when the user contacts the compact detergent containing one or more of the aforesaid substances with the fabric to be washed and the water.
  • the development of ammonia and/or of oxygen and/or of chlorine occurs in the most favorable conditions, both from the physical-chemical point of view as well as from the point of view of performance, as the developing of ammonia and/or of oxygen, and/or the chlorine are directly contacting, in high concentration, the fabric to be washed.
  • the mixer is started and operated for about minutes.
  • the mixture of the powders is discharged into the feeding hopper of a hammer-type mill.
  • the mill is fitted with sieves suitable to obtain a maximum grain size of 100 mesh is started.
  • the powder thus milled is pounded into the feeding hopper of the dosing group of the compacting machine.
  • the dosing group is pre-set for dosages of 250 grams, with dosing allowable variations of :5 grams.
  • the compacting machine is started, feeding the lubricating devices of the dies and of the molds with a mixture, in equal parts of ventilated talcum and silica gel.
  • the dosed powder, poured into the lubricated dies, is de-aerated by compression and then definitely compacted in the actual compacting station under a 155 kg./sq. cm.
  • the compacted piece will be expelled in the subsequent station and sent to a packaging station.
  • the mixture of powders is discharged into the feeding hopper of the hammer mill.
  • the mill fitted with suitable sieves in order to obtain a grain size of 120 mesh is started.
  • the so mixed powder is transferred to the feeding powder of the dosing group of the compacting machine.
  • the dosing group is pre-set for dosages of 400 grams, with allowable variations of i8 grams.
  • the compacting machine is started, supplying the lubricating devices of the dies and of the molds with a mixture in equal parts of fluid vaseline oil and of fluid silicone.
  • the dosed powder, poured in the lubricated dies, will be deaerated by compression and then finally compacted in the actual compacting station under a 180 kg./sq. cm. pressure.
  • the compacted piece will be expelled in the subsequent station and sent to a packaging station.
  • the product is to be used as a toilet soap, of course the composition of the possible formulations will be different, even if the manufacturing process remains identical to that described in the first part of the present invention.
  • compositions there will be ingredients well known in the techniques of toilet soap and cosmetic art, such as for instance sodium lauryl-sulphate, sulphates from animal or vegetable fats, alkyl-aryl-sulphonates, as detergents particularly suitable for the skin, fatting agents as for instance lanolin or vaseline, foaming agents, such as for instance the ethoxylated or non-ethoxylated fat amides, ingredients for imparting a particular plasticity to the finished piece such as for instance talcum or silica gel, waterglass having the features similar to those previously cited in connection with the manufactured product for washing purposes, and finally eccipients, coloring agents, and perfume.
  • ingredients well known in the techniques of toilet soap and cosmetic art such as for instance sodium lauryl-sulphate, sulphates from animal or vegetable fats, alkyl-aryl-sulphonates, as detergents particularly suitable for the skin, fatting agents as for instance lanolin or vaseline, foaming agents, such as for instance the ethoxylated or
  • a remarkable advantage of these kinds of soap is the possibility of obtaining a product which, when in solution, can have a neutral pH or an acid pH thus showing a beneficial effect on the skin which normally has an acid pH.
  • This is possible as the above cited detergents (as generally almost all synthetic detergents) are stable in acid medium, as opposed to the behavior of common soap from fatty acids which is unstable in acid medium.
  • an organic acid can be added to the formulation, such as for instance citric acid and/or tartaric acid and/or oxalic acid; or it is possible to use a buffer system such as for instance a mixture of monosodic and bisodic phosphates, or buffer mixtures of other well known complexed phosphates.
  • a buffer system such as for instance a mixture of monosodic and bisodic phosphates, or buffer mixtures of other well known complexed phosphates.
  • other buffer systems can be used, provided they are compatible with the other components of the formulation.
  • the compacted piece is expelled in the subsequent station and sent to a packaging station.
  • These grains can be obtained by means of the well known dry or wet grain making processes and can have any detergent and/or bleaching and/or cleaning composition, previously mixed with a coloring agent.
  • a process for preparing a dry, compacted detergent composition comprising dry mixing the components of the detergent composition which are:
  • detergent composition further contains at least one member of the group consisting of sodium perborate and sodium percarbonate.
  • the detergent composition further contains at least one member of the group consisting of dichloroisocyanuric acid, trichloroisocyanuric acid, alkaline earth metal salts thereof, lithium hypochlorite and calcium hypochlorite.

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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)
US625411A 1966-03-24 1967-03-23 Process for preparing a dry compacted detergent composition Expired - Lifetime US3562165A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IT3126466 1966-03-24
IT665966 1966-03-24

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US3562165A true US3562165A (en) 1971-02-09

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US (1) US3562165A (show.php)
JP (1) JPS4817447B1 (show.php)
DE (1) DE1617040A1 (show.php)
ES (1) ES338432A1 (show.php)
GB (1) GB1175749A (show.php)

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4219436A (en) * 1977-06-01 1980-08-26 The Procter & Gamble Company High density, high alkalinity dishwashing detergent tablet
US4242216A (en) * 1979-09-27 1980-12-30 Chemed Corporation Stabilized dichlorodimethyl hydantoin
US4281421A (en) * 1979-03-12 1981-08-04 The Procter & Gamble Company Passive dosing dispenser with improved hypochlorite cake
US4390441A (en) * 1980-04-11 1983-06-28 Lever Brothers Company Machine dishwashing composition
US4847089A (en) * 1986-07-16 1989-07-11 David N. Kramer Cleansing and distinfecting compositions, including bleaching agents, and sponges and other applicators incorporating the same
US5096609A (en) * 1990-02-15 1992-03-17 Hoechst Aktiengesellschaft Detergent containing sodium disilicate having a water content of 0.3 to 6% by weight
US5552079A (en) * 1993-09-13 1996-09-03 Diversey Corporation Tableted detergent, method of manufacture and use
WO1999020734A1 (en) * 1997-10-23 1999-04-29 The Procter & Gamble Company Laundry bars having improved physical properties
WO1999020732A1 (en) * 1997-10-23 1999-04-29 The Procter & Gamble Company Laundry bars having improved physical properties
US20060091356A1 (en) * 2004-10-28 2006-05-04 Pickens Stanley R Calcium hypochlorite composition
EP1133548B2 (en) † 1998-11-27 2006-07-12 Unilever Plc Detergent compositions in tablet form
EP2190969A4 (en) * 2007-05-04 2011-05-04 Ecolab Inc Pressed, self-hardening, solid cleaners and method of preparation therefor
US8647567B2 (en) 2011-04-06 2014-02-11 The Clorox Company Methods of providing uniform delivery of a functional agent from a shaped composition
ITMI20130391A1 (it) * 2013-03-15 2014-09-16 Euroacque S R L Ricambio per dosatori proporzionali di polifosfato
US9862915B2 (en) 2007-10-18 2018-01-09 Ecolab Usa Inc. Pressed, self-solidifying, solid cleaning compositions and methods of making them
US10457902B2 (en) 2008-01-04 2019-10-29 Ecolab Usa Inc. Solid tablet unit dose oven cleaner

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0005286A1 (en) * 1978-04-18 1979-11-14 THE PROCTER & GAMBLE COMPANY Compact solid disinfecting composition containing a mixture of lithium hypochlorite and calcium hypochlorite
US4309299A (en) * 1980-09-04 1982-01-05 Lever Brothers Company Detergent composition having improved chlorine retention characteristic and method of making same
GB8830010D0 (en) * 1988-12-22 1989-02-15 Unilever Plc Detergent composition
FR2649090A1 (en) * 1989-06-30 1991-01-04 Barvil Sarl Cartridge for disinfecting water, especially in a swimming pool
GB8926642D0 (en) * 1989-11-24 1990-01-17 Unilever Plc Detergent composition
GB9123058D0 (en) * 1991-10-30 1991-12-18 Unilever Plc Detergent composition

Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4219436A (en) * 1977-06-01 1980-08-26 The Procter & Gamble Company High density, high alkalinity dishwashing detergent tablet
US4281421A (en) * 1979-03-12 1981-08-04 The Procter & Gamble Company Passive dosing dispenser with improved hypochlorite cake
US4242216A (en) * 1979-09-27 1980-12-30 Chemed Corporation Stabilized dichlorodimethyl hydantoin
US4390441A (en) * 1980-04-11 1983-06-28 Lever Brothers Company Machine dishwashing composition
US4847089A (en) * 1986-07-16 1989-07-11 David N. Kramer Cleansing and distinfecting compositions, including bleaching agents, and sponges and other applicators incorporating the same
US5096609A (en) * 1990-02-15 1992-03-17 Hoechst Aktiengesellschaft Detergent containing sodium disilicate having a water content of 0.3 to 6% by weight
US5552079A (en) * 1993-09-13 1996-09-03 Diversey Corporation Tableted detergent, method of manufacture and use
WO1999020734A1 (en) * 1997-10-23 1999-04-29 The Procter & Gamble Company Laundry bars having improved physical properties
WO1999020732A1 (en) * 1997-10-23 1999-04-29 The Procter & Gamble Company Laundry bars having improved physical properties
WO1999020733A1 (en) * 1997-10-23 1999-04-29 The Procter & Gamble Company Laundry bars having improved physical properties
EP1133548B2 (en) † 1998-11-27 2006-07-12 Unilever Plc Detergent compositions in tablet form
US20060091356A1 (en) * 2004-10-28 2006-05-04 Pickens Stanley R Calcium hypochlorite composition
US7465412B2 (en) * 2004-10-28 2008-12-16 Ppg Industries Ohio, Inc. Calcium hypochlorite composition
EP2190969A4 (en) * 2007-05-04 2011-05-04 Ecolab Inc Pressed, self-hardening, solid cleaners and method of preparation therefor
US9862915B2 (en) 2007-10-18 2018-01-09 Ecolab Usa Inc. Pressed, self-solidifying, solid cleaning compositions and methods of making them
US11104869B2 (en) 2007-10-18 2021-08-31 Ecolab Usa Inc. Pressed, self-solidifying, solid cleaning compositions and methods of making them
US12467020B2 (en) 2007-10-18 2025-11-11 Ecolab Usa Inc. Pressed, self-solidifying, solid cleaning compositions and methods of making them
US10457902B2 (en) 2008-01-04 2019-10-29 Ecolab Usa Inc. Solid tablet unit dose oven cleaner
US8647567B2 (en) 2011-04-06 2014-02-11 The Clorox Company Methods of providing uniform delivery of a functional agent from a shaped composition
US8920743B2 (en) 2011-04-06 2014-12-30 The Clorox Company Faucet mountable water conditioning devices
US8955536B2 (en) 2011-04-06 2015-02-17 The Clorox Company Faucet mountable water conditioning systems
ITMI20130391A1 (it) * 2013-03-15 2014-09-16 Euroacque S R L Ricambio per dosatori proporzionali di polifosfato

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Publication number Publication date
DE1617040A1 (de) 1971-02-25
GB1175749A (en) 1969-12-23
JPS4817447B1 (show.php) 1973-05-29
ES338432A1 (es) 1968-06-16

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