FORM 2
THE PATENTS ACT, 1970
(39 of 1970)
COMPLETE SPECIFICATION
(See section 10; rule 13)

Title of the invention
PROCESS FOR MANUFACTURING
DETERGENT POWDER comprising a volatile compnent

HINDUSTAN LEVER LIMITED, a company incorporated under the Companies Act, 1913 of Hindustan Lever House, 165/166, Backbay Reclamation, Mumbai-400 020, State of Maharashtra, India

GRANTED
The following specification (particularly) describes the nature of this invention (and the manner in which it is to be performed)


orgn
IN/PCT/2002/00036
11-1-2002

12-1-2004/30-4-2004

Technical Field
The present invention relates to a process for manufacturing of detergent powder products comprising a volatile component and apparatus for the production thereof.
Background
Detergent powder products are well known commercial products in the laundry care industry. For example, such detergent products have been sold under the brand names Wisk (Unilever) and Tide (Procter & Gamble) in the USA have been available for many years.
Processes for manufacturing detergent powder products are also well known. In a typical process, a base powder formulation is passed through several steps wherein one or more detergent components and/or adjuncts are added in one or more post-dosing steps. These components and/or adjuncts can include, for example, perfumes, enzymes and colorants. It is not uncommon for commercial detergent powder products that are marketed and sold under different brand names to have a common base powder, yet be different because they have different components and/or adjuncts post-dosed to the common base powder. For example, brand A may have perfume X and enzyme Y, while brand B has perfume Z and no enzyme. It is also not uncommon for a single plant to be used to make several brands, even though those brands are unique. This can present scheduling issues because, for purposes of safety and quality control, it must be ensured that there is no cross contamination between the brands.

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When manufacturing detergent powder products, it has been found that a significant amount of post-dosed material can be lost prior to final packaging, particularly volatile components such as perfumes. This is generally due the type of processes used in the manufacture of detergent powder products and the manner in which agents are applied to the base powder. Typically, one or more component(s) and/or adjunct(s) in a detergent powder product are incorporated into the product by post-dosing the component(s) and/or adjunct(s) as particulate material to a base powder. This generally necessitates one or more mixing steps to ensure good distribution of the post-dosed material in the base powder.
With reference to Fig. 1, a prior art process for manufacturing detergent powder products is shown. Base powder 100 flows from storage vessel 10 onto weigh feeder 20. Belt 22 moves the powder across weigh feeder 20, causing base powder 100 to cascade off belt 22 into vessel 30. Flow rates of base powder 100 can range from about 15,000 lbs/hr (e.g. about 6,500 kg/hr) to about 100,000 lbs/hr (e.g. about 45,500 kg/hr). As powder 100 falls towards vessel 30, pressurized spray system 40 sprays liquid perfume P onto the powder, designated as powder 100P in vessel 30. Spray system 40 can include tank 42 containing perfume P, pressure pump. 44 and spray nozzle 46. The rate of perfume application from pressurized spray system 40 is coordinated with the rate of flow of powder to ensure uniform dosing. Levels of perfume in the final product is typically in the range of from about 0.1 wt % to about 0.5 wt %.

Prom vessel 30, powder 100P is transferred to post dosing belt 50, wherein belt 50 further transfers the perfumed powder towards mixer 60, which is preferably a fluidized bed. Prior to entering mixer 60, various miscellaneous agents M2, M4 and M6 are added to powder 100P via vessels 62, 64 and 66, respectively. Agents that can be added to the powder moving along post dosing belt 50 include enzymes, colorants, sulfates, carbonates and other known additives. Typically, between 5 wt % and 25 wt % of the final powder composition can be added in this process. After addition of the miscellaneous agents, the powder is mixed in mixer 60 to ensure uniformity and is designated as 100P+M.
After mixer 60, powder 100P+M is transferred to vessel 70. Vessel 70 is preferably a hopper and serves to transfer powder 100P+M to one or more weigh flasks 80. The weigh flasks then gravity dispense a known quantity of powder (based on a weight measurement) 100P+M into suitable containers 90, such as boxes, bottles, buckets or bags.
Several inefficiencies can be identified with the process of Fig. 1, all relating to the application of perfume between weigh feeder 20 and vessel 30. First, the relatively high rate of powder flow from weigh feeder 20 requires a correspondingly high rate of flow of perfume from pressurized spray system 40. This can result not only in inefficient and uneven application of the perfume that can further result in clumps of powder 100P, but misapplied spray can accumulate on belt 22, hopper 30 and other equipment in the area. Second, when powder 100P travels along post dosing belt 50, at least some quantity of perfume volatilizes. Third, when powder enters mixer 60, the action within the mixer causes further loss of perfume, particularly if fluidized bed technology is utilized.

Fourth, because between about 5 wt % to about 25 wt % of the final product is added after application of the perfume, the amount of perfume, ori a weight percent (wt %) basis is higher for powder 100P than for powder 100P+M. This tends to exacerbate the above-identified inefficiencies. Fifth, when production of a first variant having a first perfume is complete and a second variant with a second perfume is to be manufactured, the production line must be cleaned from weigh feed 20 forward. Similarly, because the perfume is introduced early in the process and is able to enter the atmosphere at several steps, it is generally not..possible to. simultaneously run other variants in the same plant, for purposes of quality control. Lastly, losing perfume to the atmosphere results in economic and environmental costs.
Therefore, there is a need for an improved detergent powder-product manufacturing process wherein the loss of perfume and other volatile actives during the process of making_ the
powder is minimized. There is also a need to ensure
uniformity of the final packaged product. There is a
further need to increase plant efficiency.

Perfume agents can be classified by their relative volatility. High volatile perfumes are also known as "high notes" while relatively non-volatile perfume are also known
i— ■ as "low notes." High note perfumes are typically more
perceptible by humans than low note perfumes, which is
believed to be due to their high volatility. Known high
notes also have a wider range of odors and, therefore, allow
for greater f1exibi1ity when selecting perfume agents.
Unfortunately, when manufacturing detergent powder product,
it is the desired high notes that are typically lost during
processing. This has resulted in a decreased amount of high
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note perfumes being used and, if used, less make it into the packaged product. Therefore, there is also a need for a detergent powder product manufacturing process that would allow for increased usage of high note perfumes, wherein the highly volatile perfumes are retained in the powder so as to reach the consumer.
Definition of the Invention
The present disclosure relates to a process which minimizes the loss of perfume and other volatile agents during the manufacture of detergent powder product. It has been found that it is possible to rearrange the order of addition or inclusion of volatile agents from one or more of the manufacturing process steps. More specifically, by adding the perfume and/or other volatile agents closer to the step of packaging, there is loss of the perfume to the atmosphere during the process. In the case of perfumes, the perfume profile remains relatively unaltered and a wider variety of perfumes can be used.
Thus, in a first aspect, the present invention provides a process for manufacturing a detergent powder product comprising a volatile component said process comprising mixing a base powder with one or more detergent components and/or adjuncts in a mixing apparatus to produce a base powder mixture and applying a volatile component after the mixing apparatus to the base powder mixture.
In a second aspect, the present invention provides an apparatus for applying a volatile component to a mixture
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comprising a base powder and one or more detergent
components and/or adjuncts comprising:
(i) measuring means for measuring a pre-determined amount
of the mixture; (ii) container moving means for sequentially moving
containers underneath the measuring means; and (iii) a spray nozzle disposed (1) above the container
moving means and (2) at least partially below a
portion of the measuring means. DETAILED DESCRIPTION OF THE INVENTION
Definitions
Hereinafter, in the context of this invention, the term "detergent powder product" encompasses substantially finished products for sale. Preferably, the detergent powder product contains detergent-active material such as synthetic surfactant and/or soap at a level of at least 5 wt%, preferably at least 10 wt% of the product.
Hereinafter, in the context of this invention, the term "base powder" is a powder comprising at least one component of the detergent powder product of which it forms a part and which accounts for at least 20 wt % of the detergent powder product. In a preferred embodiment, the base powder comprises at least two components of the detergent powder product of which it forms a part.
Preferably, the base powder accounts for at least 25 wt%, more preferably at least 3 0 wt% and yet more preferably at least 3 5 wt% of the detergent powder product. Of course, the base powder may account for 50 wt% or more, e.g. 75 wt%,
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of the detergent powder product. In particular, this can be the case when the base powder contains larger number of components.
In order to obtain a detergent powder product from a base powder, the base powder must be post-dosed with or to other detergent components or adjuncts or any other form of detergent admixture. Thus a base powder as herein defined may, or may not contain detergent-active material such as synthetic surfactant and/or soap. The minimum requirement is that it should contain at least one material of a general kind of conventional component of detergent powder products, such as a surfactant (including soap), a builder, a bleach or bleach-system component, an enzyme, an enzyme stabiliser or a component of an enzyme stabilising system, a soil anti-redeposition agent, a fluorescer or optical brightener, an anti-corrosion agent or an anti-foam material.
In a preferred embodiment of this invention, the base powder contains detergent-active material such as synthetic surfactant and/or soap at a level of at least 5 wt%, preferably at least 10 wt% of the product.
In another preferred embodiment of this invention, the base powder comprises a detergency builder.
In yet another preferred embodiment, the base powder is a direct product of a granulation process. As used herein, the term "granulation" refers to a process in which at least two components of a detergent powder product, which exist as separate raw materials, which can be in solid (e.g. particulate) or liquid form, are formed into granules by an appropriate granulation technique. Suitable granulation techniques are well known to the skilled person and include

spray-drying and non-spray drying mechanical mixing techniques, e.g. agglomeration.
Detergent compositions and ingredients
As previously indicated, the detergent powder product prepared by the process of the invention is substantially a fully formulated detergent composition. This section relates to final, fully formed detergent compositions.
The total amount of detergency builder in detergent powder product is suitably from 10 to 80 wt%, preferably from 15 to 60 wt%. The builder may be present in an adjunct with other components or, if desired, separate builder particles containing one or more builder materials may be employed.
Suitable builders include hydratable salts, preferably in substantial amounts such as at least 25% by weight of the solid component, preferably at least 10% by weight. Hydratable solids include inorganic sulphates and carbonates, as well as inorganic phosphate builders, for example, sodium orthophosphate, pyrophosphate and tripolyphosphate.
Other inorganic builders that may be present include sodium carbonate (as mentioned above, an example of a hydratable solid), if desired in combination with a crystallisation seed for calcium carbonate as disclosed in GB-A-1 437 950. As mentioned above, such sodium carbonate may be the residue of an inorganic alkaline neutralising agent used to form an anionic surfactant in situ.

Organic builders that may be present include polycarboxylate polymers such as polyacrylates, acrylic/maleic copolymers, and acrylic phosphin'ates; monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono-, di-and trisuccinates, carboxymethyloxysuccinates, carboxymethyloxymalonates, dipicolinates,
hydroxyethyliminodiacetates, aminopolycarboxylates such as nitrilotriacetates (NTA), ethylenediaminetetraacetate (EDTA) and iminodiacetates, alkyl- and alkenylmalonates and succinates; and sulphonated fatty acid salts. A copolymer of maleic acid, acrylic acid and vinyl acetate is especially preferred as it is biodegradable and thus environmentally desirable. This list is not intended to be exhaustive.
Especially preferred organic builders are citrates, suitably used in amounts of from 2 to 30 wt%, preferably from 5 to 25 wt%; and acrylic polymers, more especially acrylic/maleic copolymers, suitably used in amounts of from 0.5 to 15 wt%, preferably from 1 to 10 wt%. The builder is preferably present in alkali metal salt, especially sodium salt, form.
Crystalline and amorphous aluminosilicate builders may also be used, for example zeolites as disclosed in GB-A-1 473 201; amorphous aluminosilicates as disclosed in GB-A-1 473 202; and mixed crystalline/amorphous aluminosilicates as disclosed in GB 1 470 250; and layered silicates as disclosed in EP-B-164 514.
Aluminosilicates, whether used as layering agents and/or incorporated in the bulk of the particles may suitably be present in a total amount of from 10 to 60 wt% and preferably an amount of from 15 to 50 wt% based on the final detergent composition. The zeolite used in most commercial particulate detergent compositions is zeolite A.
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Advantageously, however, maximum aluminium zeolite P (zeolite MAP) described and claimed in EP-A-384 070 may be used. Zeolite MAP is an alkali metal aluminosilicate of the P type having a silicone to aluminium ratio not exceeding 1.33, preferably not exceeding 1.15, and more preferably not exceeding 1.07.
The detergent powder product preferably contains one or more detergent-active compounds which may be chosen from soap and non-soap anionic, cationic, nonionic, amphoteric and zwitterionic surfactants, and mixtures thereof. Many suitable detergent-active compounds are available and are fully described in the literature, for example, in "Surface-Active Agents and Detergents", Volumes I and II, by Schwartz, Perry and Berch. The preferred detergent-active compounds that can be used are soaps and synthetic non-soap anionic and nonionic compounds.
Anionic surfactants are well-known to those skilled in the art. Examples include alkylbenzene sulphonates, particularly linear alkylbenzene sulphonates having an alkyl chain length of C8-C15; primary and secondary alkyl sulphates, particularly C12-C15 primary alkyl sulphates; alkyl ether sulphates; olefin sulphonates; alkyl xylene sulphonates; dialkyl sulphosuccinates; and fatty acid ester sulphonates. Sodium salts are generally preferred.
Nonionic surfactants that may be used include the primary and secondary alcohol ethoxylates, especially the C8-C20 aliphatic alcohols ethyxylated with an average of from 1 to 20 moles ethylene oxide per mole of alcohol, and more
especially the C10-C15 primary and secondary aliphatic alcohols ethoxylated with an average of from 1 to 10 moles
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of ethylene oxide per mole of alcohol. Non-ethoxylated nonionic surfactants include alkylpolyglycosides, glycerol monoethers, and polyhydroxyamides (glucamide).
The total amount of surfactant present in the detergent powder product is suitably from to 5 to 40 wt% although amounts outside this range may be employed as desired.
The detergent powder product may also contain a bleach system, desirably a peroxy bleach compound, for example, an inorganic persalt or organic peroxyacid, capable of yielding hydrogen peroxide in aqueous solution. The peroxy bleach compound may be used in conjunction with a bleach activator (bleach precursor) to improve bleaching action at low wash temperatures. An especially preferred bleach system comprises a peroxy bleach compound (preferably sodium percarbonate optionally together with a bleach activator), and a transition metal bleach catalyst as described and claimed in EP-A-458 397 and EP-A-509 787.
Usually, any bleach and other sensitive ingredients, such as enzymes and perfumes, will be post-dosed to the base powder, e.g. after granulation, along with other minor ingredients.
Typical minor ingredients include sodium silicate; corrosion inhibitors including silicates; antiredeposition agents such as cellulosic polymers; fluorescers; inorganic salts such as sodium sulphate, lather control agents or lather boosters as appropriate; proteolytic and lipolytic enzymes; dyes; coloured speckles; perfumes; foam controllers; and fabric softening compounds. This list is not intended to be exhaustive.
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Fig. 2 illustrates an improved detergent powder product manufacturing process;
Fig. 3 illustrates an alternate, improved detergent powder product manufacturing process;
Fig. 4 illustrates a preferred location for placing a perfume applicator;
Fig. 5 illustrates an alternate, preferred location for placing a perfume applicator; and
Fig. 6 illustrates an alternate, preferred location for placing a perfume applicator.
Detailed Description of the drawings
For simplicity, "perfume" will be used herein to describe an ingredient that can volatilize in an undesirable manner. It is within the scope of the present disclosure, however, that other volatile agents can be advantageously applied by the presently disclosed process. These agents can include, for example, water, surfactants, dye transfer inhibitors, hygene agents and other volatile agents.
With reference to Fig. 2, a process is shown that is similar to that in Fig. 1. The primary modification illustrated in Fig. 2 is the elimination of the step of applying perfume prior to mixer 60. More specifically, perfume applicator system 40 has been eliminated. Subsequent to mixer 60, however, the perfume is now applied using perfume system 100. Perfume system 100 applies perfume P to powder 100M just prior to packaging. As shown, powder 100M exits vessel

70 and enters weigh flask 80. In a preferred process, weigh flasks 80 are filled with an amount of powder that corresponds to a predetermined weight amount.
Alternatively, volumetric measurement can be used. After the proper amount of powder has entered flasks 80, the flasks open to release the powder into containers 90. As shown, the perfume is preferably applied to the powder between flasks 80 and containers 90. However, it is within the scope of the present disclosure that perfume can be applied at any point subsequent to mixer 60, i.e., prior to vessel 70 or prior to weigh flasks 80. Referring back to Fig. 2, the preferred method of applying the perfume is through spray application. In a most preferred method, ultra-sonic spray applicators are utilized, such as those available from Sono-Tek Corporation located in Milton, New York.
Pilot tests of the above-described process and apparatus of Fig. 2 have produced commercially acceptable perfumed detergent powder product.
Turning now to Fig. 3, an alternative improved detergent powder product manufacturing process is shown. Apparatus of 200 of Fig. 3 is a rotary filler machine. With reference to Fig. 2, this apparatus would replace that which is shown subsequent to vessel 70, i.e., powder 100M would be transported to rotary filler 200 for subsequent filling into final containers. Rotary filler 200 includes a plurality of filling stations 210 that preferably rotate in a clockwise direction so as to alternately dispose filling stations 210 over containers 220. Ultra-sonic spray nozzles 230 are shown associated with each filling station 210. Alternately, it is possible to mount a single, stationary spray applicator at
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the location of the powder transfer to containers 220 and have that applicator apply perfume or other volatile liquids as each filling station rotates into place. This would eliminate the need for multiple perfume applicators. Turning to Fig. 4, a cross sectional view of the Fig. 3 filling apparatus is shown. Filling station 210 is shown having support 240 holding funnel section 250. Spray applicator 230 is mounted to a lower portion of funnel 250 so as to direct perfume onto powder 100M after it falls through funnel 250 into and before entering box 220. Box 220 is directed along conveyer 255 to facilitate the filling process. In a most preferred embodiment, volumetric or weight measurement signals would control the amount of powder that falls through funnel 250 into container 220. By knowing the amount of powder to be placed in each container, the desired amount of volatile substance can be applied.
Turning to Figs. 5 and 6, alternate preferred embodiments of mounting spray nozzles 230 to a rotary filling process are disclosed. With reference to Fig. 5, spray nozzle 230 is attached to the base of funnel 250 and sprays through orifice 260 in funnel 250. Alternatively, with reference to Fig. 6, the end of the spray nozzle can be mounted within funnel 250. In either of the embodiments of Figs. 5 and 6, the spray nozzle 230 can be mounted at any point along the funnel, i.e., it need not be at the bottom of funnel 250.
By applying some or all of the perfume towards the end of the process, significantly less perfume is lost to the atmosphere. In addition, by decreasing the amount of perfume that is lost to the atmosphere, a wider variety of perfume agents can be retained on the final product. For example, significant amounts of perfumes having a relatively high volatility, until now, would be lost to the atmosphere
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and not make it to the final boxed product. However, by the present procedure, high note volatility perfumes can be included in the detergent powder product and delivered to the customer. This process, therefore, allows for a much greater variety of perfumes to be used. Also, as indicated above, other volatile agents can be applied using the process described herein. The processes described herein also allows for greater manufacturing efficiency and flexibility by adding product specific volatile agents towards the end of the process. With this processing advantage, cleaning requirements are reduced and common base powders (100+M) can be manufactured and stored in bulk for later packaging.


We claim:
1. A process for manufacturing detergent powder comprising a volatile component-
providing detergent base powder;
providing an apparatus for mixing the base powder;
transferring the base powder to the mixing apparatus;
mixing the base powder in the mixing apparatus;
transferring the base powder to a packaging apparatus
thereafter weighing the base powder in amounts suitable for filling in individual
product containers;
providing a volatile ingredient; and
applying the volatile ingredient to the weighed base powder prior to releasing the
powder into final individual product containers.
2. The process as claimed in claim 1, wherein the step of providing the volatile
ingredient comprises providing at least one perfume ingredient.
3. The process as claimed in claim 1, wherein the step of providing the mixing
apparatus comprises providing a fluidized bed.
4. The process as claimed in claim 1, wherein the step of applying the volatile
ingredient comprises providing atleast one spray nozzle and using the at least one
spray nozzle to apply the volatile ingredient to the detergent base powder.
5. The process as claimed in claim 4, wherein the step of providing the at least one
spray nozzle comprises providing at least one ultra-sonic spray nozzle.

Dated this 11th day of January 2002
Dr. Sanchita ganguli of S.Majumdar & Co. Applicant's agent

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