EP0019413B1 - Process for manufacture of coloured detergents speckles - Google Patents

Process for manufacture of coloured detergents speckles Download PDF

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Publication number
EP0019413B1
EP0019413B1 EP80301488A EP80301488A EP0019413B1 EP 0019413 B1 EP0019413 B1 EP 0019413B1 EP 80301488 A EP80301488 A EP 80301488A EP 80301488 A EP80301488 A EP 80301488A EP 0019413 B1 EP0019413 B1 EP 0019413B1
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EP
European Patent Office
Prior art keywords
speckles
accordance
surfactant
coloured
colourant
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
Application number
EP80301488A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0019413A1 (en
Inventor
Giovanni Pagani
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.)
Unilever PLC
Unilever NV
Original Assignee
Unilever PLC
Unilever NV
Priority date (The priority date 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 date listed.)
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Publication date
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Application filed by Unilever PLC, Unilever NV filed Critical Unilever PLC
Publication of EP0019413A1 publication Critical patent/EP0019413A1/en
Application granted granted Critical
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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
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • 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
    • C11D3/40—Dyes ; Pigments

Definitions

  • This invention relates to a process for the production of coloured speckles for use in a washing powder and to the speckles obtained by the process.
  • Coloured speckles are considered by manu- facturerers to be desirable components of washing powders since there is a substantial body of evidence that customers prefer speckled powders to plain ones.
  • speckles of the correct size and size distribution so that they have the desired appearance in a white powder, and to obtain them of the desired density so that they do not segregate from the body of the powder, is not at all easy.
  • speckles Many methods of making speckles have been suggested. The simplest is perhaps that in which a portion of the spray-dried powder, or a component of it such as sodium tripolyphosphate, is sprayed with a colourant solution. That is not really satisfactory because the larger, visible particles become unevenly coloured and because a high proportion of finely-divided coloured material is produced which imparts a slight overall hue to the powder, whereas what is required is a white powder.
  • Spray-drying of coloured crutcher slurries is a second method which has been suggested but although this produces satisfactory speckles, the process itself is inconvenient in that the spray-drying tower needs to be cleaned after each batch of speckles is prepared, interrupting production.
  • the process of the invention permits the preparation of speckles which are entirely phosphate-free, which is desirable for regions in which local laws prohibit the sale of washing powder containing phosphate.
  • the speckles can be prepared from any surfactant which has a melting point sufficiently high for it to be liquefied and solidified again to form a solid material, such as a flake or a bead, at room temperature.
  • a surfactant which has a melting point sufficiently high for it to be liquefied and solidified again to form a solid material, such as a flake or a bead, at room temperature.
  • tallow alcohol ethoxylated with an average of 25 moles of ethylene oxide per mole of alcohol hereafter referred to as tallow alcohol 25EO
  • tallow alcohol 25EO tallow alcohol ethoxylated with an average of 25 moles of ethylene oxide per mole of alcohol
  • other surfactants can be used.
  • the melting points of nonionic surfactants are somewhat molecular weight dependent and also dependent on the degree of branching in the hydrophobic part of the molecule.
  • Straight chain primary alcohols in the C 12 -c l range begin to be sufficiently solid to be used in the process of the invention when they are ethoxylated with about 10 moles of ethylene oxide per mole of alcohol. More highly branched alcohols have lower melting points and very much higher molecular weights must be reached before sufficiently solid materials for use in the invention are encountered.
  • anionic surfactants which are fusible and solid at room temperature can be used in this invention.
  • examples of these are sodium dodecylbenzene sulphonate and sodium primary alkyl sulphates.
  • the surfactant preferably has a melting point of above 35°C and more preferably between 40°C and 80°C.
  • the nature of the colourant is not critical, provided that it does not interact significantly with any of the components of the powder.
  • the speckles can be prepared in any colour desired although darker colours make more visual impact than light ones. Blue is a particularly preferred colour for speckles since the colourant can then serve as a blue whitener in the formulation. Formulations containing the blue- whitener Polar Billiant Blue GAW C.I. Acid Blue 127:1 have been described, and this material is particularly preferred as a colourant for use in the invention.
  • Preferred levels of colourant in the speckles are from 0.01 to 0.20% by weight, preferably 0.05 to 0.15% by weight.
  • the step (b) in the process in accordance with the invention may be carried out in any manner which leads to the formation of solid material, either in the form of granules or in the form of a continuous or discontinuous film.
  • the preferred manner of performing this step is to spray a molten mixture of colourant and surfactant onto a rotating drum through which coolant passes. Solidified material is then scraped off the surface of the drum by a knife, normally situated diametrically opposite to the point where the spraying takes place. In this way coloured flakes of surfactant are produced.
  • the flakes are milled to produce speckles of the desired size.
  • the optimum diameter for speckles made by the process of this invention is below 15000 l im, preferably between 500 and 1500 jM m.
  • the solid flake material can be milled in any manner, a particularly preferred manner of carrying out this step is to use a hammer mill. This type of mill is described in more detail below, but it consists essentially of a comminuting device and a sieving device. The sieve size can be altered to suit the process in hand, although only the upper size limit can be controlled. There is no control over the amount of fines material which is produced.
  • the final stage of the process is a separation stage.
  • speckles of the desired size produced by milling of the coloured, spray- cooled flake material are separated from extraneous material, principally more finely divided material than is required, by an elutriation technique.
  • Elutriation is a known technique for classifying particular material which has been found especially suitable for use in the present process. It is described generally on page 899 of the book "Chemical Engineering” referred to later. Basically, the technique consists in blowing a stream of air up a column and introducing unclassified solid material into the column via a side tube. The air stream carries the more buoyant (and therefore smaller) particles away, leaving the heavier ones behind. In our application of the technique the velocity of the air stream is adjustable so that the fraction of extraneous solid material which is carried away can be controlled.
  • the elutriation column is transparent so that a visual check can be kept upon the transport phenomena inside.
  • the apparatus consists of a closed cylindrical vessel (10) fitted with heating coils (11) and a stirrer (12).
  • the upper end of the vessel (10) is provided with two inlets, one for nonionic surfactant and one for dyestuff, these being shown schematically.
  • the lower end of the vessel is provided with an outlet, also shown schematically, for coloured molten nonionic surfactant and the outlet leads to a pump (13) connected to a head (14).
  • the head is arranged above a drum (15).
  • Supports (16) carry a hollow shaft (17) on the major axis of the drum by means of bearings (not shown), arranged so that the shaft and drum are rotatable together.
  • the shaft is hollow and has the double function of carrying the drum and also conducting cooling water to the inside of it.
  • a knife edge (18) is arranged substantially tangentially to the drum so that the edge almost touches the surface thereof and both the drum and the knife edge are positioned vertically above a large funnel (19) provided with an outlet (20).
  • the outlet communicates with the feed (21) of a hammer mill (22) which is an important component of the apparatus of the invention.
  • a hammer mill as is known to those skilled in the art, consists of a screen, above which a high speed rotating disc is provided to which are fixed a number of hammer bars which are swung outwards by centrifugal force. Two designs of such mills are illustrated on pages 883 and 884 of "Chemical Engineering", volume 2, by J M Coulson and J F Richardson, published by Pergammon Press, Oxford, in 1962.
  • the output from the hammer mill shown schematically is connected by line (23) to a cyclone separator (24) which has a gas/vapour outlet (25) and a solids outlet (26), the latter communicating with an elutriation column (27) which is transparent.
  • the elutriation column is connected through filter column (28) and manometer valve (29) to a pump (30).
  • granules of tallow alcohol 25EO are placed in the cylindrical vessel (10) and hot water is passed through the heating coils (11).
  • the stirrer is turned on and when a sufficiently high temperature has been reached to liquefy the nonionic surfactant, a dyestuff, such as Polar Brilliant Blue GAW, is injected into the molten mass, either in powdered form or predispersed in a liquid nonionic surfactant.
  • the mixture is stirred until homogeneous and is then pumped out of vessel (12) by pump (13) and discharges through head (14).
  • the liquid mixture falls onto the surface of the rotating drum (15) which is cooled below the melting point of the coloured tallow alcohol 25EO by cold water passed into the drum through the hollow shaft (17).
  • the liquid mixture consequently solidifies into a film which is scraped off the surface of the drum by the knife-edge (16) diagonally opposite the head.
  • the solid material which is scraped off falls into the funnel (19) and passes out through outlet (20) through the inlet (21) of the hammer mill (22). In the mill the solid material is milled to a maximum average diameter of 1400 ⁇ rn and air lifted through line (23) to the cyclone separator.
  • the solid particles separated by the cyclone are fed into the elutriation column (26). Air is sucked into the column between its base and the funnel (31) by pump (30). The pressure and hence the velocity of the air can be measured and controlled by the manometer/valve (29).
  • the particles in the size range 500 to 1400 ⁇ m are weighed in the weighing pan (32) and stored until required in storage container (34). Alternatively they can be fed directly into the storage container (35).
  • the speckles produced by the process of the invention are clearly visible in the powder and do not segregate from it.

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)
  • Developing Agents For Electrophotography (AREA)
  • Glanulating (AREA)
EP80301488A 1979-05-09 1980-05-07 Process for manufacture of coloured detergents speckles Expired EP0019413B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB7915957 1979-05-09
GB7915957 1979-05-09

Publications (2)

Publication Number Publication Date
EP0019413A1 EP0019413A1 (en) 1980-11-26
EP0019413B1 true EP0019413B1 (en) 1982-01-20

Family

ID=10505020

Family Applications (1)

Application Number Title Priority Date Filing Date
EP80301488A Expired EP0019413B1 (en) 1979-05-09 1980-05-07 Process for manufacture of coloured detergents speckles

Country Status (9)

Country Link
EP (1) EP0019413B1 (cs)
AT (1) ATE590T1 (cs)
AU (1) AU539128B2 (cs)
BR (1) BR8002744A (cs)
DE (1) DE3060147D1 (cs)
ES (1) ES491306A0 (cs)
GR (1) GR66803B (cs)
IT (1) IT1121458B (cs)
PT (1) PT71203B (cs)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2343456A (en) * 1998-11-06 2000-05-10 Procter & Gamble Speckle particles and compositions containing the speckle particles

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU470133B2 (en) * 1972-04-06 1976-03-04 Colgate-Palmolive Company, The Detergent compositions
DE2632367C2 (de) * 1975-07-23 1986-03-27 The Procter & Gamble Co., Cincinnati, Ohio Granulierte gefärbte Partikel
CA1111736A (en) * 1977-05-31 1981-11-03 Enrique C. Robles Process for preparing coloured detergent flakes

Also Published As

Publication number Publication date
IT7968410A0 (it) 1979-07-05
EP0019413A1 (en) 1980-11-26
PT71203B (en) 1981-09-17
ES8104396A1 (es) 1981-04-01
BR8002744A (pt) 1980-12-16
DE3060147D1 (en) 1982-03-04
GR66803B (cs) 1981-03-29
PT71203A (en) 1980-06-01
AU539128B2 (en) 1984-09-13
AU5817780A (en) 1980-11-13
ES491306A0 (es) 1981-04-01
ATE590T1 (de) 1982-02-15
IT1121458B (it) 1986-04-02

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