CN112041417B

CN112041417B - Detergent particles

Info

Publication number: CN112041417B
Application number: CN201880092648.2A
Authority: CN
Inventors: 徐丹; 沈睿; 田晓; 关喆; 黄旭
Original assignee: Procter and Gamble Co
Current assignee: Procter and Gamble Co
Priority date: 2018-05-10
Filing date: 2018-05-10
Publication date: 2022-07-29
Anticipated expiration: 2038-05-10
Also published as: EP3790950A1; CN112041417A; EP3790950B1; WO2019213890A1; MX2020011976A

Abstract

A detergent particle is characterized by a median particle size in the range of 200 to 1000 μm and an aspect ratio of not more than 2, and contains 85 to 95 wt.% of C having a branched or linear chain that is not alkoxylated ₆ ‑C ₁₆ An Alkyl Sulfate (AS) of an alkyl group and 4 to 14 wt% of a water-soluble salt, wherein the water or water content is 1 to 5 wt%.

Description

Detergent granules

Technical Field

The present invention relates to detergent granules useful in the manufacture of cleaning products, especially granular detergent products.

Background

Has been found to have C ₆ -C ₁₆ The mid-cut alkyl sulphate of branched or unbranched un-alkoxylated alkyl groups (MCAS or AS) is effective in foam boosting when used AS a co-surfactant with linear alkyl benzene sulphonate (LAS) in cleaning compositions, especially laundry detergent compositions. For example, WO2009010911 discloses MCAS for promoting foaming and forming detergent compositions with reduced total surfactant content in LAS-based surfactant systems, but without significant deteriorationUse of the sudsing profile of a detergent composition.

Some MCAS feedstock may be obtained in the form of elongated needles formed by an extrusion process. This extruded needle form of MCAS material is easy to process and has little or no risk of caking, agglomeration or plugging of the production line. However, extruded MCAS needles have limited foam boosting effect when used in combination with LAS in cleaning compositions, possibly due to their relatively large size and corresponding poor dissolution characteristics.

The MCAS feedstock may be obtained in the form of a fine powder having a median particle size in the range of 200 to 1000 μm, which shows good suds boosting effect when used as a co-surfactant for LAS. However, due to the phase change of the MCAS surfactant and its tendency to absorb ambient water when placed in a humid environment, such MCAS fines tend to agglomerate at temperatures above 35-37 ℃ and can cause significant processing challenges during transportation and manufacturing.

There is therefore a need to provide MCAS particles with physical properties and chemical composition which on the one hand allow an improved balance between good dissolution characteristics and satisfactory foam boosting effect and on the other hand allow an improved balance between reduced risk of agglomeration and ease of processing/handling.

Disclosure of Invention

The present inventors have surprisingly and unexpectedly found that by producing detergent particles having a relatively small particle size and a relatively low aspect ratio (i.e. which are more spherical than acicular in shape), the dissolution characteristics of such detergent particles can be improved and the suds boosting effect correspondingly enhanced. Furthermore, when such detergent particles contain a very high level (e.g., about 85% to about 95% by weight) of MCAS in combination with a sufficient amount (e.g., about 4% to about 14% by weight) of water-soluble salts, they are less likely to absorb ambient water and thus less likely to cake or form lumps during transport or storage.

In one aspect, the present invention relates to a detergent granule comprising:

a) from about 85% to about 95%, by weight of the detergent particle, of an Alkyl Sulfate (AS) having a branched or straight chain non-alkoxylated alkyl group containing from about 6 to about 16 carbon atoms;

b) from about 4% to about 14%, by weight of the detergent particle, of a water soluble salt selected from the group consisting of sodium sulfate, sodium carbonate, magnesium chloride, magnesium sulfate, sodium silicate, and combinations thereof; and

c) from about 1% to about 5% by weight of the detergent granule of water,

while the detergent particles are characterized by a median particle size in the range of from about 200 μm to about 1000 μm and an aspect ratio of no more than about 2.

In another aspect, the present invention relates to cleaning compositions comprising from about 0.1% to about 10%, by weight of such cleaning compositions, of the detergent particles described above.

In another aspect, the present invention relates to the use of the above cleaning composition for hand washing of fabrics.

These and other aspects of the invention will become more apparent upon reading the following detailed description of the invention.

Drawings

Fig. 1 is a graph showing the dynamic vapour absorption data of detergent particles of the invention according to an embodiment of the invention and comparative detergent particles outside the scope of the invention.

Detailed Description

The features and advantages of various embodiments of the present invention will become apparent from the following description, which includes examples intended to give a broad representation of specific embodiments of the invention. Various modifications will be apparent to those skilled in the art from this description and from practice of the invention. The scope of the present invention is not intended to be limited to the particular forms disclosed, and the invention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the claims.

As used herein, articles such as "a" and "an" when used in a claim are understood to mean one or more of what is claimed or described. The terms "comprising", "containing", "including" and "including" are meant to be non-limiting.

As used herein, the term "detergent particle" refers to a particle containing one or more detersive actives including, but not limited to, surfactants, bleaching agents, enzymes, polymers, chelating agents, and combinations thereof.

As used herein, unless otherwise indicated, the term "cleaning composition" includes multipurpose or "heavy duty" detergents, especially cleaning detergents for fabrics, in granular or powder form, as well as cleaning adjuncts such as bleaching agents, rinse aids, additives or pretreatment types; hand dishwashing agents or light duty dishwashing agents, especially those of the high sudsing type; machine dishwashing detergent; mouthwashes, denture cleaners, car or carpet cleaners, bathroom cleaners; hair shampoos and hair rinses; shower gels and foam baths and metal cleaners; and cleaning aids such as bleach additives or pre-treatment types. In a preferred aspect, the cleaning composition is a solid laundry detergent composition, and more preferably a free-flowing particulate laundry detergent composition (i.e., a particulate laundry detergent product).

As used herein, the term "median particle size" refers to the midpoint of the particle size distribution of the detergent particles, as measured by the sieve test as disclosed herein.

As used herein, the term "aspect ratio" refers to the ratio of the largest diameter of an article to the smallest diameter of such article that is orthogonal to the largest diameter.

As used herein, the term "water soluble" refers to a solubility of greater than about 30 grams per liter (g/L) of deionized water measured at 20 ℃ and atmospheric pressure.

As used herein, the term "consisting essentially of …" means that the composition contains less than about 1%, preferably less than about 0.5%, of ingredients other than those listed.

In addition, the terms "substantially free", or "substantially free" mean that the indicated material is present in an amount of from 0 wt% to about 0.5 wt%, or preferably from 0 wt% to about 0.1 wt%, or more preferably from 0 wt% to about 0.01 wt%, and most preferably it is not present at analytically detectable levels. The term "substantially pure" or "substantially pure" means that the indicated material is present in an amount of about 99.5% to about 100% by weight, preferably about 99.9% to about 100% by weight, and more preferably 99.99% to about 100% by weight, and most preferably all other materials are present only as impurities below analytically detectable levels.

MCAS

The AS surfactant used in the detergent particles of the present invention comprises a branched or straight chain non-alkoxylated alkyl group containing from about 6 to about 16 carbon atoms and is therefore also referred to AS mid-cut AS or MCAS.

Preferably, AS has the formula R-O-SO ₃ ^- M ⁺ Wherein R is branched or straight chain non-alkoxylated C ₆ -C ₁₆ An alkyl group, and M is an alkali metal cation, an alkaline earth metal cation, or an ammonium cation. More preferably, the R group of the AS surfactant contains from about 8 to about 14 carbon atoms, more preferably from about 10 to about 14 carbon atoms, and most preferably from about 12 to about 14 carbon atoms. R may be substituted or unsubstituted, and is preferably unsubstituted. R does not substantially have any degree of alkoxylation. M is preferably a sodium cation, a potassium cation, or a magnesium cation, and more preferably M is a sodium cation.

Preferably, but not necessarily, the detergent particles of the present invention contain C ₆ -C ₁₆ Mixtures of AS surfactants, wherein C ₈ -C ₁₄ The AS surfactant is present in an amount ranging from about 85% to about 100% by total weight of the mixture. This mixture may be referred to as "C-rich ₈ -C ₁₄ AS mixture ". More preferably, such C-rich ₈ -C ₁₄ The AS mixture contains about 90 wt% to about 100 wt%, or 92 wt% to about 98 wt%, or about 94 wt% to about 96 wt%, or 100(i.e., pure) C by weight ₈ -C ₁₄ AS。

In a particularly preferred embodiment of the invention, the detergent granule comprises a detergent having from about 30 wt% to about 100 wt% or from about 50 wt% to about 99 wt%, preferably from about 60 wt% to about 95 wt%, more preferably from about 65 wt% to about 90 wt%, and most preferably from about 70 wt% to about 80 wt% C ₁₂ C of AS ₆ -C ₁₆ A mixture of AS surfactants. Furthermore, such C ₆ -C ₁₆ The mixture of AS surfactants may contain from about 10% to about 100%, preferably from 15% to about 50%, and more preferably from 20% to about 30%, by weight of C ₁₄ And (6) the AS. This mixture may be referred to as "C-rich ₁₂ -C ₁₄ AS mixture ".

In a most preferred embodiment of the invention, the detergent granule comprises a blend of essentially C ₁₂ And/or C ₁₄ AS surfactant a mixture of AS surfactants. For example, such mixtures of AS surfactants may consist essentially of from about 70% to about 80% by weight of C ₁₂ AS and 20 to about 30 wt.% of C ₁₄ AS composition with little or no other surfactant. Such mixtures may also be prepared from substantially pure C ₁₂ AS, or alternatively substantially pure C ₁₄ And (3) the AS.

Commercially available AS mixtures which are particularly suitable for carrying out the invention are

V95G, available from Cognis (Monheim, Germany).

Furthermore, the detergent particles of the present invention may contain C ₆ -C ₁₆ Mixtures of AS surfactants comprising more than about 50 wt.%, preferably more than about 60 wt.%, more preferably more than 70 wt.% or 80 wt.%, and most preferably more than 90 wt.% or even 100 wt.% (i.e., substantially pure) of a linear AS surfactant having an even number of carbon atoms, including, for example, C ₆ 、C ₈ 、C ₁₀ 、C ₁₂ 、C ₁₄ And C ₁₆ An AS surfactant.

As described for C ₆ -C ₁₆ Mixtures of AS surfactants can be readily obtained by sulfonating alcohols having the corresponding number of carbon atoms. The desired distribution of carbon chain lengths can be obtained by using alcohols with a corresponding distribution of chain lengths, prepared synthetically or by extraction/purification from natural raw materials, or formed by mixing corresponding pure starting materials. E.g. C ₆ -C ₁₆ Mixtures of AS surfactants can be derived from naturally occurring triglycerides (such AS those contained in palm kernel oil or coconut oil) AS follows: such triglycerides are chemically treated to form a mixture of long chain alcohols, and then such alcohols are sulfonated to form AS surfactants. Mixtures of alcohols derived from naturally occurring triglycerides typically contain greater than about 20 wt.% C ₁₆ -C ₁₆ An alcohol. In order to form the desired C as described above ₆ -C ₁₆ Mixtures of AS surfactants, possibly separated from the initial mixture before the sulphonation step, containing a lower proportion of C ₁₆ -C ₁₆ A mixture of alcohols. Alternatively, desired C ₆ -C ₁₆ Mixtures of AS surfactants can be readily obtained by isolating and purifying the formed AS mixture. Suitable methods of isolation and purification include, but are not limited to: distillation, centrifugation, recrystallization and chromatographic separation.

The amount of AS surfactant present in the detergent particles of the present invention may range from about 85 wt% to about 95 wt%, and preferably from about 88 wt% to about 92 wt%, based on the total weight of the composition. With such a high level of one or more AS surfactants, the detergent particles of the present invention exhibit high detersive activity and very good dissolution characteristics. In a most preferred embodiment of the present invention, the cleaning composition contains from about 85% to about 95%, preferably from about 88% to about 92%, by weight of an AS mixture consisting essentially of from about 70% to about 80%, by weight, C ₁₂ AS and 20 to about 30 wt.% of C ₁₄ And (3) the AS.

Detergent particles with higher surfactant content are generally expected to be more difficult to handle due to their tendency to absorb more water. Thus, it has been surprisingly and unexpectedly found that the detergent particles of the present invention, although containing such high levels of one or more AS surfactants, actually absorb less water at different Relative Humidities (RH) in the range of 40% to 80% compared to detergent particles containing lower amounts of AS surfactant, for example less than about 85% by weight. Accordingly, the detergent particles of the present invention are less likely to agglomerate or agglomerate and are easier to handle during storage or transport.

Water-soluble salt

The water soluble salts used in the detergent particles of the present invention may be selected from sodium sulphate, sodium carbonate, magnesium chloride, magnesium sulphate, sodium silicate, and combinations thereof. Preferably, the water soluble salt is selected from sodium sulfate, sodium carbonate or a combination thereof.

The amount of water-soluble salts present in the detergent granules of the present invention may range from about 4 wt% to about 14 wt%, preferably from about 5 wt% to 12 wt%, and more preferably from about 6 wt% to about 10 wt%. If the detergent granule contains less than about 4% by weight of water-soluble salts, it exhibits poor flowability and is therefore more difficult to handle during storage, transport and manufacture. If the detergent particle contains more than about 14 wt% water soluble salts, the amount of AS surfactant in such detergent particles may have to be reduced to less than about 85 wt%, which is undesirable for the reasons described above.

Water content

The detergent granules of the present invention may contain from about 1 wt% to about 5 wt%, preferably from about 1.5 wt% to about 4 wt%, more preferably from about 2 wt% to about 3 wt% water. Too much water in the detergent granule can adversely affect its flowability and handleability.

Other ingredients

The detergent particles of the invention may contain one or more other ingredients such as silica, zeolites, other surfactants, enzymes, bleach actives, sequestrants, perfumes, dyes, fluorescent materials and the like.

Preferably, the detergent particles of the invention consist essentially of MCAS described above, water soluble salts and water. More preferably, the detergent particles of the present invention are substantially free of other ingredients.

Size and shape of detergent particles

The detergent particles of the present invention may be characterized by a median particle size in the range of from about 200 μm to about 1000 μm, preferably from about 250 μm to about 600 μm, more preferably from about 300 μm to about 425 μm.

Furthermore, it may be characterized by an aspect ratio of not more than 2, preferably not more than 1.5, more preferably not more than 1.2, most preferably not more than 1.1. The detergent particles of the present invention preferably have a spherical or substantially spherical shape, which serves to further improve their flowability and handleability during storage and transportation.

Cleaning composition

The detergent particles of the present invention may be used alone for cleaning, but preferably they are combined with other particles to form a cleaning composition, such as a granular laundry detergent product.

In one aspect, the detergent particles are typically added to the cleaning composition at a level of from about 0.1 wt% to about 10 wt%, preferably from about 0.2 wt% to about 8 wt%, more preferably from about 0.5 wt% to about 5 wt%, by weight of the cleaning composition. Preferably, the cleaning composition is a granular detergent composition.

The detergent particles of the present invention may be combined with other particles, such as: surfactant particles, such as anionic detersive surfactant particles (especially those containing LAS), including agglomerates and extrudates, nonionic detersive surfactant particles, including agglomerates or extrudates, and cationic detersive surfactant particles, including agglomerates and extrudates; enzyme granules; perfume particles, including agglomerates or extrudates of perfume microcapsules, and perfume encapsulates such as starch encapsulated perfume accord particles; polymer particles, including soil release polymer particles, cellulosic polymer particles; buffer particles, including carbonate and/or silicate particles, preferably particles comprising carbonate and silicate, such as sodium carbonate and sodium silicate co-particles, and particles and sodium bicarbonate; other spray-dried particles; fluorescent whitening particles; aesthetic particles such as colored stripes or needles or layered particles; bleaching particles such as percarbonate particles, especially coated percarbonate particles, including carbonate and/or sulphate coated percarbonate, silicate coated percarbonate, borosilicate coated percarbonate, sodium perborate coated percarbonate; bleach catalyst particles such as transition metal catalyst bleach particles and imine bleach boosting particles; preformed peracid particles; a hueing dye particle; and any mixtures thereof.

In addition to the detergent particles described above, it is preferred that the cleaning composition of the present invention further comprises C ₁₀ -C ₂₀ Linear alkyl benzene sulphonate (LAS) and more preferably such cleaning compositions further comprise a fatty acid or salt thereof. MCAS-containing detergent particles of the invention may interact with such LAS and fatty acid/salts to provide improved sudsing characteristics.

It may also be especially preferred that the cleaning composition comprises low levels of builder, or even is substantially free of builder. In a preferred embodiment, the cleaning composition is free of builder.

Application method

The cleaning compositions are generally used to clean and/or treat an area, especially a surface or fabric. As used herein, "surface" may include such surfaces as dishes, glass, and other cooking surfaces, hard surfaces, hair, or skin. Such methods include the steps of: embodiments of the cleaning composition (in neat form or diluted in a wash liquor) are contacted with at least a portion of a surface or fabric, and such surface or fabric is then optionally rinsed. The surface or fabric may be subjected to a washing step prior to the above-described rinsing step. For purposes of the present invention, "washing" includes, but is not limited to, scrubbing, wiping, and mechanical agitation.

The composition solution pH is selected to be most suitable for the target surface to be cleaned, among a wide range of pH spanning from about 5 to about 11. The pH of such compositions preferably has a pH of from about 5 to about 8 for personal care such as skin and hair cleansing, and from about 8 to about 10 for laundry cleaning compositions. The composition is preferably used at a concentration of about 200ppm to about 10,000ppm in solution. The water temperature is preferably in the range of about 5 ℃ to about 100 ℃.

In one aspect, a method of laundering fabrics using the cleaning compositions of the present invention is disclosed. The method may include the step of contacting the fabric to be laundered with a cleaning composition or wash liquor formed therefrom. The fabric may comprise most any fabric capable of being laundered under normal consumer use conditions.

The cleaning compositions herein are particularly useful in a hand wash environment. It can also be used in beating washing using top loading or front loading automatic washing machines.

The cleaning composition may be used at a concentration of about 500ppm to about 15,000ppm in solution, and optionally more dilute wash conditions may be used. Optionally, 50g or less, or 45g or less, or 40g or less, or 35g or less, or 30g or less, or 25g or less, or 20g or less, or even 15g or less, or even 10g or less of the cleaning composition is dissolved in water to form a wash liquor. The wash liquor preferably has a pH of about 8 to about 10.5. The wash liquor may comprise 40 litres or less of water, or 30 litres or less, or 20 litres or less, or 10 litres or less, or 8 litres or less, or even 6 litres or less of water. The wash liquor may comprise from above 0 litres to 15 litres, or 2 litres and to 12 litres, or even to 8 litres of water. In the case of dilute wash conditions, the wash liquor may comprise 150 liters or less of water, 100 liters or less of water, 60 liters or less of water, or 50 liters or less of water, especially for hand wash conditions, and may depend on the number of rinses. The water to fabric ratio is typically from about 1:1 to about 30: 1. Typically, from 0.01Kg to 2Kg of fabric per litre of wash liquor is dosed into the wash liquor.

Preferably, the cleaning composition is useful in hard water conditions, which areA mid-water hardness of between about 17ppm to about 600 ppm; or from about 34ppm to about 340 ppm; or from about 51ppm to about 300ppm hard water ions, such as Ca ²⁺ 、Mg ⁺ Etc. or such as Ca ²⁺ And Mg ²⁺ . It is also preferred that the cleaning composition be used at cold water temperatures, where the temperature is from about 5 ℃ to about 40 ℃, or from about 20 ℃ to about 30 ℃, or from about 15 ℃ to about 25 ℃, and all other combinations in the range of from about 15 ℃ to about 35 ℃, and all ranges in the range of from 10 ℃ to 40 ℃.

Test method

The following techniques must be used to determine the performance of the detergent particles and detergent compositions of the present invention so that the invention described and claimed herein can be fully understood.

Test 1: median particle size test method (sieve test method)

This test method can be used to determine the median particle size of the detergent particles of the present invention. The particle size distribution of detergent particles is measured by sieving the particles through a series of sieves of progressively decreasing size. The weight of material remaining on each sieve was then used to calculate the particle size distribution and median particle size.

This Test was performed using ASTM D502-89, "Standard Test Method for Particle Size of Soaps and Other Detergents", approved at 26.5.1989, with the addition of the sieve instructions used in the analysis, to determine the median Particle Size of the Test particles. According to section 7 "Procedure using machine-sizing method", a set of clean and dry sieves comprising U.S. Standard (ASTM E11) sieves #8(2360 μm), #12(1700 μm), #16(1180 μm), #20(850 μm), #30(600 μm), #40(425 μm), #50(300 μm), #70(212 μm) and #100(150 μm) is required. The above described set of screens is used for a given machine screening method. The detergent particles of interest were used as samples. A suitable screen shaker is available from w.s.tyler Company (Mentor, Ohio, u.s.a.) in a suitable vibratory screening machine that separates the soap particles based on their particle size using a prescribed machine-screening process. The data was plotted on a semi-logarithmic graph by plotting the micron-sized openings of each sieve against the abscissa of the logarithm and the cumulative mass percentage (Q3) against the linear ordinate.

An example of the above data Representation is given in FIG. A.4 of ISO 9276-1:1998, "reproduction of results of particulate size analysis-Part 1: Graphical reproduction". Median particle size (D) ₅₀ ) Is defined as the abscissa value at which the cumulative mass percentage equals 50 percent and is calculated by linear interpolation between data points directly above (a50) and directly below (b50) the 50% value using the following formula:

D ₅₀ ＝10[Log(D _a50 )-(Log(D _a50 )-Log(D _b5o ))*(Q _a5o -50％)/(Q _a50 -Q _bso )]

wherein Q _a50 And Q _b50 Cumulative mass percent values for data directly above and below 50 percent, respectively; and D _a50 And D _b50 Mesh micron values corresponding to these data. In the case where the 50 percent value is below the finest mesh (150 μm) or above the coarsest mesh (2360 μm), then after an geometric progression of no more than 1.5, additional screens must be added to the set until the median value falls between the two measured mesh.

And (3) testing 2: moisture content measurement

Two (2) grams of sample detergent particles were tested in a Mettler Toledo HR73 halogen moisture analyzer at 115 ℃ for 40 minutes. The percent (%) mass loss at the end of the measurement was recorded as the moisture content of the sample detergent particles.

Examples

Example 1: comparative test showing reduced Water absorption of the inventive detergent particles

Preparing two sample detergent particles, including a sample of the invention of detergent particles, containing about 88% MCAS (containing about 65% by weight of C12 material, 25% by weight of C14 material, 7% by weight of C16 material, and no more than 3% by weight of other materials), 9.5% sodium sulfate and 2.5% water, 90% MCAS and 10% sodium sulfate (within the scope of the invention), based on the total dry weight of such detergent particles; and a comparative sample of detergent particles containing 78% MCAS (same composition as above), 19.5% sodium sulphate and 2.5% water (outside the scope of the invention) by total dry weight of such detergent particles.

Each sample detergent particle was formed by adding a specific amount of sodium sulfate to a heated concentrated MCAS paste (containing 74 wt% MCAS in water) and then mixing in a temperature controlled reactor at an elevated temperature in the range of 60-80 ℃ for 10 minutes. The mixture was then spread manually onto a flat surface to form a thin layer having a thickness of about 3-10mm, which was dried in an oven at an elevated temperature of 110 ℃ for about 2 hours. Once the dried mixture reached a target moisture content of about 2-3%, it was removed from the oven and ground to powder form by using a Fritsch pulverette 14 grinder (commercially available from Fritsch GmbH (IDar-Oberstein, Germany)) at a speed setting of 6 and using a 1.5mm screen. The powder thus formed was further sieved to reach the same particle size distribution as follows:

Table 1.

The moisture adsorption isotherms for both the detergent particles of the invention and the comparative detergent particles were obtained using an SPS-11 moisture adsorption analyzer, commercially available from ProUmid GmbH & co. The measurements were started at 0% Relative Humidity (RH) and each was increased stepwise to about 80% final RH in steps of about 10% RH. The equilibrium conditions for each step were set to be constant at. + -. 0.01% by mass within 30 minutes. The temperature of the test conditions was set to 35. + -. 0.1 ℃. The delta mass (dm) at each RH% is in% which is an indicator of the percentage of water absorbed by the sample detergent particle at the corresponding RH%, calculated from the following formula:

fig. 1 is a graph plotting the delta mass (dm, in%) of a detergent particle of the present invention and the delta mass (dm, in%) of a comparative detergent particle over an RH range of about 40% to about 80% RH. Clearly, under relatively high humidity conditions (e.g., RH in the range of about 40% to about 80%), the detergent particles of the present invention absorb less water than the comparative detergent particles. Thus, the detergent particles of the present invention are less likely to cake or agglomerate when stored or transported in countries or regions where humidity may be challenging.

Example 2: comparative test showing reduced caking of detergent particles of the invention in a big bag test

Five (5) sample detergent particles comprising four (4) inventive samples of detergent particles a-E (within the scope of the invention), and one (1) comparative sample of detergent particles C1 (outside the scope of the invention) were prepared having the following composition:

TABLE 2

Each sample detergent particle was formed by the same method as described in example 1.

The big bag test is used to detect and qualitatively assess potential problems with such materials prior to shipment into the big bag, during which the materials may be exposed to elevated temperatures. During big bag testing, 100g +/-1g of test material is first placed into a plastic beaker and the top surface of the test material is ensured to be flush. The second beaker is placed into the first beaker containing the test material while the bottom of the top second beaker rests on the test material without pushing or forcing the top second beaker into the test material. The two beakers were sealed together with PVC tape. The 3Kg mass was placed in the top second beaker such that the top second beaker served as a bearing surface for the 3Kg mass on the test material. The beaker with the test material and a mass of 3Kg is then placed in an oven at 35 ℃ and 80% RH. After 20 hours under such test conditions, 3kg of material was removed and the test material was cooled to ambient temperature (1 hour minimum cooling time). The bottom first beaker containing the cooled test material was inverted to see how easily/hard the test material can flow out of the bottom first beaker. The flowability of the test material was graded using the following grading scale:

10: free flowing.

·9 ¹ / ₂ : slight pause, incomplete free flow, but no caking

9: caked, but broke up when inverted to give a powder.

·8 ¹ / ₂ : clumps, but crumbles when re-tilted several times.

8: clumps, but broken up by gentle shaking.

7: clumps, but broken up by moderate shaking.

6: caked, but broken up by vigorous shaking

5: clumps, but are broken up by vigorous shaking.

4: agglomerated solid

The following are the big bag test results for five (5) detergent granule samples:

TABLE 4

	C1	A	B	D	E
						Big bag grading score	7	9.5	9.5	9.5	9.5

The dimensions and values disclosed herein are not to be understood as being strictly limited to the exact numerical values recited. Rather, unless otherwise specified, each such dimension is intended to mean both the recited value and a functionally equivalent range surrounding that value. For example, a dimension disclosed as "40 mm" is intended to mean "about 40 mm".

Each document cited herein, including any cross referenced or related patent or patent application and any patent application or patent to which this application claims priority or its benefits, is hereby incorporated by reference in its entirety unless expressly excluded or otherwise limited. The citation of any document is not an admission that it is prior art with any disclosure of the invention or the claims herein or that it alone, or in combination with any one or more of the references, teaches, suggests or discloses any such invention. Further, to the extent that any meaning or definition of a term in this document conflicts with any meaning or definition of the same term in a document incorporated by reference, the meaning or definition assigned to that term in this document shall govern.

While particular embodiments of the present invention have been illustrated and described, it would be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.

Claims

1. A detergent granule comprising:

a) from 85% to 95% by weight of the detergent particle of an alkyl sulphate having a branched or straight chain non-alkoxylated alkyl group comprising from 6 to 16 carbon atoms;

b) from 4% to 14% by weight of the detergent particle of a water soluble salt selected from the group consisting of sodium sulfate, sodium carbonate, magnesium chloride, magnesium sulfate, sodium silicate, and combinations thereof; and

c) from 1% to 5% by weight of the detergent particle of water,

wherein the median particle size of the detergent particles is in the range of from 200 μm to 1000 μm and the aspect ratio is not more than 2.

2. The detergent particle according to claim 1, wherein the branched or straight chain non-alkoxylated alkyl group of the alkyl sulfate salt comprises from 8 to 14 carbon atoms.

3. The detergent particle according to claim 1 or 2, wherein the water soluble salt is selected from sodium sulfate, sodium carbonate, and combinations thereof.

4. The detergent particle according to claim 1, wherein the median particle size of the detergent particle is in the range of from 250 μ ι η to 600 μ ι η.

5. The detergent particle of claim 1, wherein the aspect ratio of the detergent particle is no more than 1.5.

6. A cleaning composition comprising from 0.1% to 10% by weight of the cleaning composition of a detergent particle according to any one of claims 1-5.

7. The cleaning composition of claim 6, wherein the detergent particles are present in an amount ranging from 0.2% to 8% by weight of the cleaning composition.

8. The cleaning composition of claim 6 or 7, further comprising: (1) c ₁₀ -C ₂₀ Linear alkyl benzene sulfonate; and (2) a fatty acid or a salt thereof.

9. The cleaning composition of claim 8, wherein the linear alkylbenzene sulfonate is present in an amount ranging from 6% to 15% by weight of the cleaning composition; and wherein the fatty acid or salt is present in an amount ranging from 2% to 6% by weight of the cleaning composition.

10. Use of a cleaning composition according to any of claims 6-9 for hand washing of fabrics.