KR920000113B1 - Process for preparing detergent compositions - Google Patents

Abstract

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Description

Manufacturing method of detergent composition

The present invention relates to a method for producing a high bulk density granular detergent composition having excellent cleaning ability and excellent powder properties.

Recently, in the tax supply industry, there is considerable interest in a method for producing a detergent powder having a relatively high bulk density, for example, a bulk density of 600 g / l or more. Of particular interest is the densification of spray dried powders by post treatment. For example, British Patent No. 1517713 (Unilever) discloses a method of spheronizing and isolating a detergent composition prepared by spray drying or pan granulation in a “maromerizer” (trademark) so that the bulk density is slightly increased. have.

EP 229 671A (Kao) discloses a method for continuously pulverizing and granulating a spray-drying detergent powder containing a surfactant and a builder in a high speed mixer / granulator. This granulation is carried out in the presence of an interfacial property improving agent and an optional binder. In the embodiment, the interface property improving agent is zeolite 4A (10 parts) and water (2 parts) is used together as a binder. Three parts of zeolite 4A was further mixed into the product after granulation.

In Japanese Patent No. 84 041680B (Kao), a powder of a spray-dried detergent powder is pulverized, and then a powder of sodium aluminosilicate, calcium silicate, calcium carbonate, magnesium silicate or sodium carbonate having a crystallinity of 0-100% and a particle size of 0.1-300 microns. Methods are disclosed which are mixed with granules and simultaneously or subsequently with tackifiers such as, for example, nonionic surfactants, alkylethersulfates or higher alcohols.

EP 220 024A (Procter & Gamble) discloses a method for densification of spray dried powders containing high content (30-85 wt%) of anionic surfactants. The powder is densified and then granulated with inorganic builders (sodium tripolyphosphate, or crystalline sodium aluminosilicate and sodium carbonate) added before and / or after granulation.

The present inventors now granulate the spray-dried or dry-mixed detergent base powder in a high speed mixer / granulator, and then mix the small amount of fine amorphous aluminosilicate after the granulation is completed to have a high bulk density and excellent flow characteristics. It has been found that can be prepared. For this purpose, amorphous materials are more effective in weight than crystalline zeolites.

Accordingly, the present invention provides a method for producing a granular detergent composition or component having a bulk density of 650 g / L or more, which consists of the following steps.

(i) granulating and treating particulate matter containing at least one non-soap detergent active compound and at least one inorganic builder in the presence of a liquid binder in a high speed mixer / granulator having both stirring and cutting operations. Achieving a bulkville of at least 650 g / l by densification, (ii) mixing the granular material obtained in step (i) with microcrystalline sodium aluminosilicate.

In the process of the present invention, the particulate starting material (detergent base powder) prepared by any suitable method is treated in a high speed mixer / granulator to increase bulk density and at the same time improve powder properties. The process of the present invention provides a method for producing a very dense, flockable detergent composition with excellent cleaning capabilities and good powder properties.

In the process of the present invention, granulation is carried out by a high speed mixer / granulator having both stirring and cutting operations. Preferably, the stirrer and cutter can be operated independently of each other at a rate that can be changed separately. Such a mixer can simultaneously perform a high energy stirring input and cutting action and can also be used to provide other gentle stirring regimes with or without the cutter in operation. This mixer is a versatile and flexible device.

The high speed mixer / granulator of the preferred type used in the process of the invention is in the form of a bowl and preferably has a vertical stirring axis. Especially preferred are mixers of the Fukae (trademark) FS-G series manufactured by Fukae Powtech Kogyo Co., Japan. The mixer is essentially a bowl-type vessel that can be fed through the upper passageway, with a stirrer with a vertical axis at the base and a cutter at the side wall. The stirrer and cutter can be operated at speeds that can be changed independently of one another.

hne 제품인 Diosna(상표) V 시리즈, 및 영국의 T K Fielder Ltd. 제품인 Pharma Matrix(상표)가 있다. 본 발명의 공정에 사용하기에 적합한 것으로 생각되는 기타 유사혼합기로는 일본의 Fuji Sangyo CO.제품인 Fuji(상표) VG-C 시리즈, 및 이탈리아의 Zanchetta ＆amp; Co srl 제품인 Roto(상표)가 있다.Another mixer known to be suitable for use in the process of the invention is the German Dierks & S

hne Diosna (R) V series, and TK Fielder Ltd. of the United Kingdom. Product Pharma Matrix (trademark). Other quasi-mixers believed to be suitable for use in the process of the present invention include Fuji (trademark) VG-C series manufactured by Fuji Sangyo CO. Of Japan, and Zanchetta & Roto (trademark), a Co srl product.

Another mixer suitable for use in the process of the present invention is Scotland's Morton Machine Co. Ltd's Lodige (TM) FM series of batch mixers. This mixer differs from the mixer described above in that the stirrer has a horizontal axis.

The use of a high speed mixer / granulator as described above is essential to the process of the present invention to achieve granulation and densification. In some cases, the mixer may be used in a pretreatment step before granulation is performed.

It is also within the scope of the present invention to prepare, for example, particulate particulate materials by mixing them at least partially in a high speed mixer / granulator. That is, the dry mix starting powder can be prepared from the raw materials in the high speed mixer / granulator. Alternatively, one or more additional ingredients may be mixed with a premixed powder prepared by a separate method (eg spray drying). Suitable stirring / cutting regimes and durations are selected depending on the materials to be mixed.

Another possible pretreatment that can be carried out in a high speed mixer / granulator is grinding. Whether this is necessary or not depends on the preparation of the starting powder and the free water content. For example, powders produced by spray drying may require grinding rather than powders prepared by dry mixing.

The flexibility of the device also makes it possible to select a suitable stirring / cutting regime. In general, relatively high speeds are selected for stirrers and cutters. The duration is relatively short (eg 2-4 minutes per 35 kg of batch).

The basic feature of the process of the invention is the granulation step. In this step very high densification of at least 650 g / l, preferably at least 700 g / l is achieved to provide a dense granular product with a very uniform particle size and usually spherical in shape.

Granulation is achieved by operating the mixer at a relatively high speed using a stirrer and a cutter. The duration is sufficient for a relatively short time (eg 5-8 minutes per 35 kg of batch). The final bulk density can be controlled by the choice of duration, and it has been found that the powder properties of the resulting granules are undesirable when the bulk density does not increase above 650 g / l.

The presence of the liquid binder is essential for successful granulation. The amount of the binder added should preferably not exceed the amount required for the free moisture content of the composition to be about 6 wt%. The higher the content of the binder, the lower the flow characteristics of the final granules. A binder, preferably water, can be added during or prior to the granulation process if desired, but some starting powders originally have sufficient moisture. If a liquid binder is added, it is sprayed while the mixer is in operation. One of the preferred methods is to first add the binder while operating the mixer at a relatively low speed and then increase the speed of the mixer to effect granulation.

If the starting powder has sufficient free moisture to eliminate the addition of binder, it is carried out in one step without separate grinding and granulation processes, if necessary. In this case, there is no need to determine in advance whether or not a grinding process is required. In other words, generally required mixer conditions are the same for milling and granulation, thus allowing the mixer to perform simply what is needed.

According to the present invention, after completion of the granulation process, the granular material is mixed with fine amorphous sodium aluminosilicate. When the granules are in a high speed mixer / granulator it is advantageous to add amorphous sodium aluminosilicate and to operate the mixer at a short time low speed. At this stage no further granulation takes place. It is also within the scope of the present invention to transfer the granules to another device and then add amorphous sodium aluminosilicate to it.

The granulation step is preferably carried out at a somewhat controlled temperature above ambient temperature, preferably above 30 ° C. Appropriate temperatures will obviously depend on the composition but are usually on the order of 30-45 ° C., preferably about 35 ° C. This temperature is maintained during the mixing process of the fine amorphous sodium aluminosilicate.

The amorphous sodium aluminosilicate used in the process of the present invention is a microparticulate material. Preferred average particle sizes are 0.1-20 microns, more preferably 1-10 microns. Suitable materials can be purchased under the name Alusil ™ from Crosfield Chemicals Ltd. of Warrington, Cheshire.

Amorphous sodium aluminosilicate is advantageously used in an amount of 0.2-5.0 wt%, more preferably 0.5-3.0 wt%, based on the starting material.

This material is effective at improving flow characteristics even at very low contents and also has an effect of increasing bulk density. Therefore, it is possible to control the bulk density by appropriately selecting the amount of amorphous aluminosilicate added after the granulation step.

The amorphous material used in the process of the present invention should be distinguished from the zeolite (hydrated crystalline sodium aluminosilicate) which has less weight effect in the scope of the present invention. A content higher than this amount is required before any comparable flow benefit or bulk density advantage is observed.

The process of the present invention can be used to densify and improve detergent powders prepared by any top or non-top method, such as spray drying or dry mixing. If desired, the particulate starting material can be prepared at least in part by mixing in the high speed mixer / granulator itself. This particulate starting material contains at least part of the spray dried powder.

The process of the present invention provides satisfactory results, particularly with detergent base powders containing low to medium surfactants and relatively high content of inorganic builders.

According to a first preferred embodiment of the invention this process is used for the production of high bulk density powders containing high content of sodium aluminosilicate. Such powders preferably contain up to 5 wt% phosphate builders, more preferably little phosphate builders.

Preferred starting powders contain the following components.

(a) 5-35wt% soap-free detergent active material

(b) 28-45 wt% (anhydrous basis) of crystalline or amorphous sodium aluminosilicate

Wherein the weight ratio of (b) to (a) is greater than or equal to 0.9: 1 and is 100wt% with any other detergent components.

The process of the present invention is particularly suitable for producing high bulk density powders containing medium surfactants and high zeolite content as described in our same dated application (Case C.3235). This powder contains the following components.

(a) 17-35 wt% of a non-soap detergent active material containing at least a portion of an anionic detergent active material

(b) 28-45 wt% of crystalline or amorphous sodium aluminosilicate (based on anhydride)

Wherein the weight ratio of (b) to (a) is in the range of 0.9: 1-2.6: 1 and is 100 wt% with any other detergent components.

The aluminosilicate builders present in the starting material are crystalline or amorphous or mixed and have the following general formula:

0.8-1.5 Na ₂ O. Al ₂ O ₃ . 0.8-6 SiO ₂

This material contains some bound water and needs to have a calcium ion exchange capacity of at least about 50 mg Cao / g. Preferred aluminosilicates have 1.5-3.5SiO ₂ units (in the general formula above) and have a particle size of about 100 microns or less and preferably about 20 microns or less. Amorphous and crystalline aluminosilicates can be readily prepared by the reaction of sodium silicate with sodium aluminate, as fully described in the literature.

Crystalline aluminosilicates (zeolites) are preferred for starting powders containing little or no phosphate treated by the process of the present invention. Suitable materials are described, for example, in British Patent 1 473 201 (Henkel) and British Patent 1 429 143 (Procter & Gamble). Preferred sodium aluminosilicates in this form are the well known zeolites A and X and mixtures thereof which are commercially available. 4A zeolite is particularly preferred.

In the starting powder, the ratio of aluminosilicate builder (based on anhydride) to total soap-free surfactant is preferably in the range of 1.2: 1 to 1.8: 1.

According to a second preferred embodiment of the present invention this process is a high bulk containing a significant amount of water soluble inorganic salts comprising sodium tripolyphosphate and / or sodium carbonate as described in our same dated application (Case 'C. 3261). It is used for preparation of powder of density.

Preferred starting powders contain the following ingredients.

(x) 12-70wt% non-soap detergent active material

(y) 15 wt% or more of water-soluble inorganic salts including sodium tripolyphosphate and / or sodium carbonate

The weight ratio of (x) to (y) is preferably 0.4: 1-9: 1, more preferably 1: 1: 1-9: 1. Particularly preferred starting powders contain 15-70 wt% of water-soluble inorganic salts, more preferably 15-50 wt%, in particular 20-40 wt% of sodium tripolyphosphate.

In the first and second preferred embodiments of the present invention, the soapless surfactant present in the starting powder preferably contains at least partially anionic surfactant. Suitable anionic surfactants are well known to those skilled in the art and include, for example, linear alkylbenzenesulfonates, especially sodium linear alkylbenzenesulfonates having C ₈ -C ₁₅ alkyl groups; Primary and secondary alkyl sulfates, especially C ₁₂ -C ₁₅ primary alkyl sulfates; Alkyl ether sulfate; Alpha-olefins and internal olefin sulfonates; Alkanesulfonates; Dialkyl sulfosuccinates; Fatty acid ester sulfonate; And combinations thereof.

If desired, the starting material may contain a nonionic surfactant. Nonionic surfactants are well known to those skilled in the art and include primary and secondary alcohol ethoxylates, especially C ₁₂ -C ₁₅ primary and ethoxylated with an average of 3-20 moles of ethylene oxide per mole of alcohol and There are second grade alcohols.

Preferably the surfactant component of the starting material consists of 0-70 wt%, preferably 8-60 wt%, of anionic surfactant, 0-20 wt% of preferably 0-10 wt% of nonionic surfactant.

Other forms of non-soap surfactants, such as cationic, zwitterionic amphoteric or semipolar surfactants, may also be included if desired. Many suitable detergent actives are commercially available and described in detail in the literature (eg, “Surface-Active Agents and Detergents”, Volumes I and II, by Schwartz, Perry and Berch).

If desired, soap may be included to provide foam control and additional cleaning and builder capabilities. Soap is not contained at the surfactant content levels described above.

The final granules have a bulk density of at least 650 g / l, preferably at least 700 g / l. The final granules are also characterized by particularly low levels of particle porosity that do not exceed 0.25, preferably 0.20. This distinguishes it from powders of the highest density made only by spray drying.

The final granules can be used as complete detergent composition itself. Alternatively, it may be mixed with other ingredients prepared separately or mixtures thereof to occupy the upper part or a small part of the final product. In general, the final product is made by mixing the granules with additives such as enzymes, bleaches and flavorings which are not suitable for the granulation process.

For example, detergent base powders are prepared by spray drying an aqueous slurry of ingredients that are heat resistant and compatible with each other. If necessary, the other ingredients can then be mixed here. The resulting powder is densified and granulated according to the present invention. If necessary, additional ingredients may be mixed after granulation. The densified granules usually comprise 40-100 wt% of the final product.

Alternatively, one or more raw materials and / or one or more raw material premixes may be dry mixed in the high speed mixer / granulator itself or in another apparatus to prepare a detergent base powder, followed by densification and granulation Let's do it. If necessary, additional ingredients are added after granulation.

The granules prepared according to the invention may also be "additives" which contain a relatively high content of detergent active on the inorganic carrier. In this case, a small amount is mixed with other ingredients to produce the final product.

The present invention will now be described in detail by the following non-limiting examples, unless stated otherwise percentages and parts are by weight.

Example 1

By spray drying the aqueous slurry was prepared a bulk composition of 350g / L detergent composition having the following composition.

It should be noted that the ratio of zeolite (anhydride) to non-soap surfactant in this composition is 1.59.

25 kg of this spray dried powder was placed in a high speed mixer / granulator Fukae FS-G series and ground for 4 minutes at 32 ° C. at a high speed (180 rpm agitator, 3013 rpm cutter). The mixer was then maintained at a temperature of 35 ° C. and water (500 g, 2.5%) was sprayed over 0.5 minutes while operating at a slow speed (stirrer 100 rpm, cutter 3000 rpm). Granulation was then performed by operating the mixer at agitator speed 140 rpm, cutter speed 2700 rpm, temperature 36-37 ° C.

After the granulation process was completed, Asilic® (250 g, 1%), fine amorphous sodium aluminosilicate, was placed in a Fukae mixer and operated at low speed (agitator 90 rpm, cutter 300 rpm) for 1 minute. The product thus obtained was not fluid and did not tend to agglomerate. The properties of this product and the properties of the samples before adding alusil are shown in Table 1 below.

The final average particle size after alusyl addition is slightly less than before alusyl addition. This shows that some granulation reduction occurred during the treatment. Surprisingly, however, the percentage of microparticles was reduced. It is noteworthy that the bulk density is actually increased by the addition of alusil.

TABLE 1

EXAMPLE 2 & 3]

[Comparative Example A & B]

In this experiment, the effect of the addition of alusil after granulation and the effect of the addition of crystalline zeolite 4A after granulation were compared. The spray-dried powder sample used in Example 1 was treated in a Fukae mixer as described in Example 1, and alusil or zeolite was added after completion of granulation as shown in Table 2 below.

TABLE 2

It is noteworthy that there are significant differences in bulk density and dynamic flow rates.

Example 4

This experiment illustrates the manufacture of the finished world product using the process of the present invention. By spray drying the aqueous slurry was prepared a detergent composition having a free moisture content of almost zero having the following composition.

It should be noted that the ratio of zeolite (anhydride) to non-soap surfactant in this composition is 1.46.

35 kg of this spray dried powder was placed in a high speed mixer / granulator Fukae (R) FS-G series and ground at high speed for 2-4 minutes. The mixer was then stopped, sprayed with water (2.0 parts) and then run at low speed again for 5-8 minutes while maintaining the temperature at about 35 ° C. Granulation was performed in this process.

Granulation product samples were recovered from a Fukae mixer. It was not fluid and did not tend to lump. The dynamic flow rate of this product was 65 ml / s.

1.0 part of Asilyl (TM), fine amorphous sodium aluminosilicate, was placed in a Fukae mixer and operated at low speed for 1 minute. The granulated product thus obtained was not fluid and did not tend to agglomerate. The bulk density of this product was 740 g / l, the particle porosity was 405 microns and the dynamic flow rate was 105 ml / s. The following ingredients were then mixed into the granulated material to produce 100 parts of final detergent powder.

Pigment Peckle 1.5 parts

Enzyme (alkaline) 0.61 part

0.25 parts fragrance

Example 5

Comparative Example C

dige(상표) FM 시리즈안에 넣고 4분 동안 분쇄시켰다. 그 다음 혼합기를 같은 속도로 작동시키면서 물(1.1kg, 3.5%)을 분무시켰다. 그 다음 3분 더 작동시키면서 약 35℃로 유지시켜다. 이 혼합기로부터 샘플(비교 실시예 C)을 회수하였으며 이 샘플의 특성은 표 3에 나타내었다.35 kg of the spray dried powder used in Example 4 was mixed with a high speed mixer / granulator L.

Dige (TM) was put into FM series and ground for 4 minutes. Then water (1.1 kg, 3.5%) was sprayed while running the mixer at the same speed. It is then kept at about 35 ° C for three more minutes of operation. A sample (Comparative Example C) was recovered from this mixer and the properties of this sample are shown in Table 3.

1.2 kg of fine amorphous sodium aluminosilicate, Asilyl (R) was placed in a mixer and run for a further 0.5 minutes. The properties of the powder thus obtained (Example 5) are shown in Table 3, which clearly shows the advantage of adding a flow aid after the granulation is complete. The presence of alusil increased the content of microparticles <180 microns, but not an unacceptable increase.

Comparative Example D

dige(상표) FM 시리즈안에 넣고 4분동안 분쇄시켰다. 그 다음 이 혼합기안에 미세 무정형 알루미노규산나트륨인 알루실(상표) 1.2kg을 넣었다. 혼합기를 계속 작동시키면서 물(1.1kg, 3.5%)을 분무시킨 다음, 혼합기를 약 3분간 더 작동시키면서 약 35℃ 온도를 유지시켰다. 이 과정에서 과립화가 이루어졌다. 이렇게 생긴 분말의 특성은 표 3에 나타내었으며, 이로부터 과립화 이전에 알루실을 첨가하면 좋지 못한 결과가 일어난다는 것을 확실히 알 수 있었다. 미세입자 함량의 증가는 알루실을 과립화 이전에 첨가시켰을때 상당히 크다는 사실을 주목해야 한다.28.8 kg of the spray dried powder used in Example 4 was mixed with a high speed mixer / granulator L.

Dige (TM) was put into the FM series and ground for 4 minutes. Then 1.2 kg of Asilyl (TM), fine amorphous sodium aluminosilicate, was placed in the mixer. Water (1.1 kg, 3.5%) was sprayed while the mixer was running continuously, then the mixer was held for about 3 minutes while maintaining the temperature at about 35 ° C. Granulation took place in the process. The properties of the powder thus obtained are shown in Table 3, from which it can be clearly seen that the addition of alusil prior to granulation results in poor results. It should be noted that the increase in microparticle content is quite large when alusil is added prior to granulation.

TABLE 3

Comparative Example E

Same as the method of Comparative Example D, except that alusil was added before but not after grinding. Grinding and granulation were carried out as in the previous example, but the resulting product had a dynamic flow rate of zero.

Example 6

Comparative Example F

20 kg of the spray dried powder used in Example 4 was placed in a high speed mixer / granulator Fukae ™ FS-30 and ground for 4 minutes. Water (0.8 kg) was then added and the mixture granulated for 4 minutes. At this time, the temperature was maintained at about 35 ℃. A sample (Comparative Example F) was taken from this mixer and its powder characteristics were measured. The results are shown in Table 3 below.

dge 혼합기를 사용하여 얻어진 결과(비교 실시예 O)와 유사하다.Then Asilyl (TM), fine amorphous sodium aluminosilicate, was mixed. Thus, the physical properties of the raw powder (Example 6) are shown in Table 3. The result is L

similar to the results obtained using the dge mixer (Comparative Example O).

TABLE 3

Example 7

Comparative Example H

This example describes the process of densifying and granulating the powder produced by dry mixing in a high speed mixer / granulator. A composition having the following composition was prepared by mixing in a concrete mixer.

The ratio of aluminosilicate to non-soap surfactant in the mixture was 1.46. 20 kg of the composition was placed in a Diosna® V100 mixer and mixed for 1 minute at a stirrer speed of 196 rpm and a cutter speed of 3000 rpm. Water (0.2 kg) was then added for 2 minutes while the mixer was running at agitator speed 98 rpm and cutter speed 1500 rpm. This mixture was then granulated for 4 minutes at stirrer speed of 196 rpm and cutter speed of 3000 rpm. A sample (Comparative Example H) was taken and its powder properties measured (recorded below). Finally, the mixer was mixed at an agitator speed of 98 rpm and alusil (0.2 kg) was mixed without the cutter in operation. The powder properties of the final granules (Example 7) were also measured.

The powder properties before and after addition of alusyl are as follows.

Example 8

Comparative Example J

Detergent powders made of sodium tripolyphosphate were prepared by spray drying an aqueous slurry and its composition was as follows.

The ratio of water soluble crystalline inorganic salts (sodium tripolyphosphate and sodium sulfate) to soap-free surfactant was 4.6: 1.

Two separate 20 kg batches of these powders were densified in a Fukae mixer as follows. The powder was first heated at stirrer speed of 50 rpm, with no cutter running and warmed for 2-3 minutes until the temperature reached about 30-35 ° C. Then pulverized 0.5 minutes at agitator speed 180rpm, cutter speed 1000rpm. Water (0.5 wt%) was then added for 0.5 minutes while the mixer was running at stirrer speed 100 rpm and cutter speed 3000 rpm. Then, the granulation process was performed for 6 minutes at the stirrer speed of 140 rpm and the cutter speed of 3000 rpm.

In the first sample (Example 8), alusil (1.5 wt%) was added for 1 minute while operating the mixer at agitator speed 90 rpm and cutter speed 300 rpm. In the second sample (Comparative Example J), zeolite (5 wt%) was added for the same time under the same mixer conditions.

Powder characteristics are as follows.

Example 9

Comparative Example K

This example illustrates the successive addition of zeolite and alusil to densified powders.

The aqueous slurry was spray dried to prepare a detergent base powder having a content of free water of approximately 0 having the following composition.

The weight ratio of anhydrous zeolite to soap-free detergent in this base powder was 1.05: 1.

90 parts of this basic powder were granulated and densified in the same Fukae mixer as in the previous example, followed by further mixing 10 parts (based on hydrated form) of zeolite 4A. A sample (Comparative Example K) was taken and then alusil (0.4 parts) was added to form the final granules (Example 9).

The powder properties are as follows, which suggests that even if 10 parts of the zeolite has already been added afterwards, the final addition of alusil in a small amount of 0.5 parts to 100 parts significantly increases the bulk density and flow rate and decreases the tendency to agglomerate and agglomerate.

Claims (13)

A method for producing a granular detergent composition or component having a bulk density of 650 g / L or more, which comprises the following steps. (i) granulating and densifying by treating particulate material containing at least one soap-free detergent active compound and at least one inorganic builder in the presence of a liquid binder in a high speed mixer / granulator having both stirring and cutting operations. Achieving a bulk density of at least 650 g / l, (ii) mixing the granular material obtained in step (i) with fine amorphous sodium aluminosilicate. 3. A process according to claim 2 wherein the fine amorphous sodium aluminosilicate is added in an amount of 0.2-5.0 wt% of the total composition. The process according to claim 1, wherein step (ii) is also carried out in a high speed mixer / granulator. 2. A process according to claim 1, wherein the granulation is carried out in principle in a bowl-type high speed mixer / granulator with a vertical stirring shaft. The method of claim 1, wherein the particulate starting material contains at least a portion of the spray dried powder. The process according to claim 1, wherein the particulate starting material is prepared by at least partial mixing in a high speed mixer / deburper prior to the granulation step. The particulate starting material contains (a) 5-35 wt% of a non-soap detergent active material and (b) 58-45 wt% (based on anhydride) of crystalline or amorphous sodium aluminosilicate ( b) The weight ratio of (a) is 0.9: 1 or more and contains a total of 100 wt% of any other detergent component. 8. The particulate starting material of claim 7, wherein the particulate starting material comprises: (a) 17-35 wt% non-soap detergent active material containing at least a portion of the anionic detergent active material, and (b) 28-45 wt% crystalline or amorphous alumina. A process for producing sodium silicate, wherein the weight ratio of (b) to (a) is 0.9: 1 to 1-2.6: 1 and contains 100% by weight of any other cleaning ingredients. 8. A process according to claim 7, wherein the aluminosilicate (b) in the particulate starting material is a crystalline zeolite. The method of claim 1 wherein the particulate starting material contains at least 15 wt% of a water soluble crystalline inorganic salt comprising (x) 12-70 wt (y) sodium tripolyphosphate and / or sodium carbonate, and (y) versus ( The weight ratio of x) is 0.1: 1 or more and contains any other cleaning ingredients, and the total production method is characterized in that 100wt%. A process according to claim 10, wherein the weight ratio of (y) to (x) of the particulate starting material is in the range of 1: 1-9: 1. 11. A process according to claim 10, wherein the particulate starting material contains 15-70 wt% of crystalline inorganic salts including sodium tripolyphosphate and / or sodium carbonate. 11. A process according to claim 10, wherein the particulate starting material contains 15-50 wt% sodium tripolyphosphate.