JPH0768553B2 - Detergent composition and method for producing the same - Google Patents

Description

TECHNICAL FIELD The present invention relates to a high bulk density granular detergent composition having good washing performance and good powder properties, and a method for producing the same.

BACKGROUND AND PRIOR ART In recent years, within the detergent industry, relatively high, eg 600 g /
There has been considerable interest in producing detergent powders with bulk densities of liters and above. Particular attention is paid to the densification of spray-dried powders by post-treatment. In EP 219328A (Unilever), the slurry is spray dried to produce a base powder containing low to moderate levels of sodium tripolyphosphate molding agent and low levels of inorganic salts,
Produced by subsequently post-adding a solid material containing sodium sulphate of high bulk density and smaller particle size than the base powder, thus filling the cavities between the base powder particles and producing a product of high bulk density. A granular low phosphate detergent composition is shown. European Patent No. 270240A (Unilever), issued June 8, 1988, has a particle porosity of less than 0.40, anionic surfactants, optional nonionic surfactants, aluminosilicate moldings. A spray-dried phosphorus-free base powder containing an agent, a polymeric polycarboxylate and a low or zero level of electrolyte, which is preferably sodium carbonate, is shown. If desired, sodium sulfate or other small particle size and high bulk density solids may be post-added to the spray dried powder to produce a very high bulk density composition.

EP 229671A (Kao) shows that a crystalline alkaline inorganic salt, such as sodium carbonate, is post-added to the spray dried powder to produce a high bulk density product.

British Patent No. 1 517 713 (Unilever) describes a different approach, in which detergent powders produced by spray drying or pan granulation are spheronized and granulated in a "Murmelizer" (registered trademark) to obtain a bulk density. Is shown to be somewhat increased.

Japanese Patent No. 61 069 897A (Kao) has successfully pulverized and granulated a spray-dried detergent powder containing a surfactant and a molding agent in a high speed mixer / granulator.
A method is shown in which the granulation is carried out in the presence of a "surface property improving agent" and optionally a molding agent. In a high speed mixer / granulator, the spray dried powder appears to be first crushed and broken down into a fine powder. The surface modifier and optional shaping agent are then added and the finely divided material is granulated to form a high bulk density final product. Finely divided particulate solids, such as finely divided sodium aluminosilicate, are clearly necessary to prevent cheating of bowl- or cake-sized compositions. Examples of spray-dried starting powders described in Kao's specification include very high levels of surfactant (45% by weight) and relatively low levels of forming agent salts, which are cake-like. It is thought that it is very likely to become ball-shaped.

EP 220 024 A (Procter & Gamble) is also related to the densification of spray-dried powders containing high levels (30-85% by weight) of anionic surfactants. The powder is compacted and granulated, but an inorganic molding agent (sodium tripolyphosphate or sodium aluminosilicate and sodium carbonate) is added before compaction.

If the final powder is accurately formulated, especially with regard to the amount of surfactant and the ratio of surfactant to containing molding agent, without the use of "surface property improving agents" or similar finely divided substances,
The inventor has now found that, if desired, a high bulk density detergent composition can be produced by granulating the spray dried powder or dry mixed powder in a high speed mixer / granulator after micronization.

DEFINITION OF THE INVENTION First, the present invention has a bulk density of at least 650 g / liter and (a) consists at least in part of an anionic detergent active material.
-35 wt% non-soap detergent active substance, and (b) 28-45 wt% (anhydrous basis) crystalline or amorphous sodium aluminosilicate, with a weight ratio of (b) to (a) of 0.9. : 1 to 2.6: 1, preferably 1.2: 1 to 1.
Provided is a granular detergent composition which is 8: 1 and optionally added with other detergent ingredients so as to be 100% by weight.

Secondly, the invention provides a process for the preparation of a granular detergent composition or ingredient having a bulk density of at least 650 g / l, which process comprises (a) at least partly consisting of an anionic detergent active.
-35 wt% non-soap detergent active and (b) 28-45 wt% (anhydrous basis) crystalline or amorphous sodium aluminosilicate, wherein the weight ratio of (b) to (a) is at least. The presence of a liquid molding agent in a high-speed mixer / granulator having a stirring function and a cutting function, the granular starting material being 0.9: 1 and comprising 100% by weight of the granular starting material optionally added with other detergent components. Below,
However, it consists of treatment without the use of surface-improving fine-graining agents, whereby granulation and densification to a bulk density of at least 650 g / l.

Detailed Description of the Invention Product A first aspect of the present invention is a high density granular detergent powder combining high bulk density, good surface properties and excellent cleaning and cleaning performance, which is also the subject of the present invention. It can be easily and conveniently manufactured by the method.

The detergent compositions of the present invention have a moderate content of surfactants, which are at least partially anionic, and their combination of excellent properties for relatively high levels of sodium aluminosilicate forming agents and easy processability. And owe it. To properly select the absolute amounts of the powdery aluminosilicate forming agent and the surfactant, and their mutual ratios, the Japanese Patent No.
61 069897 No. A (Kao) as prescribed, without the need to use "surface property improving agents" during the granulation stage,
The inventors have discovered that the powder may be granulated in a high speed mixer / granulator. The resulting dense granules have good flow properties and are at least comparable to the compositions described in Kao containing high levels of surfactant, at least in terms of wash and wash performance and cold water dispersancy. is there.

The aluminosilicate forming agent present in the composition of the present invention may be crystalline or amorphous or a mixture thereof, and has a general formula of 0.8 to 1.5 Na ₂ O.Al ₂ O ₃ .0.8 to ₆ SiO ₂ Indicated by.

These materials contain some bound water and are required to have a calcium ion exchange capacity of at least about 50 mg CaO / g. The preferred aluminosilicate is 1.5-
It contains 3.5 SiO ₂ units (in the above formula) and has a particle size of about 100 microns or less, preferably 20 microns or less. As described in detail in the literature, amorphous aluminosilicates and crystalline aluminosilicates can be easily prepared by the reaction between sodium silicate and sodium aluminate.

In the present invention, crystalline aluminosilicate (zeolite)
Is preferably used. For example, British Patent 1 473 201 (Henkel) and British Patent 1 429 143 (Procter & Cam
ble) describes suitable substances. Preferred sodium aluminosilicates of this type are the well known commercial zeolites A and X, and mixtures thereof. Especially preferred for use in the present invention is the 4A type zeolite.

Aluminosilicate molding agent (anhydrous main component) in the composition of the present invention
The ratio of total non-soap surfactant is preferably 1.2: 1 to 1.
Within the 8: 1 range.

The included non-soap surfactant consists at least in part of an anionic surfactant. Although Suitable anionic surfactants appear to be those requiring special techniques are well known, and examples thereof include alkyl chain length linear alkyl benzene sulfonates, in particular C ₈ -C ₁₅ sodium linear alkyl benzene sulfonate having; first and second alkyl sulfates, especially C ₁₂ -C ₁₅ primary alcohol sodium sulfate; alkyl ether sulfates; alpha olefin sulfonates and internal olefin sulfonates; alkane sulfonates; Dialkyl sulfosuccinates; fatty acid ester sulfonates; and combinations thereof.

If desired, the starting powder may contain preferably small amounts of nonionic surfactants. Although it is well known that nonionic surfactants also require special technology, primary alcohol ethoxylates, especially alcohol 1
Mention may be made of C _{12 to} C ₁₅ primary alcohols and C _{12 to} C ₁₅ secondary alcohols which are ethoxylated with an average of 3 to 20 moles of ethylene oxide per mole.

The surfactant component of the compositions of the present invention may be suitably formulated with 10 to 35% by weight anionic surfactant and 0 to 10% by weight nonionic surfactant.

Other types of non-soap surfactants, such as anionic surfactants, zwitterionic surfactants, amphoteric surfactants or semi-polar surfactants may optionally be included. A large number of suitable detergent-active compounds are available, which are found in the literature, for example in "Surfactants and detergents" (Schwartz, Perry and Berch.
Co-authored, Volumes I and II).

If desired, soap may be included to provide foam control and additional detergency and molding powder. Soap is not included when the total surfactant content of the composition of the present invention is 17 to 35%.

The compositions of the invention preferably do not contain more than 5% by weight of phosphate formers, more preferably substantially zero phosphate formers.

The particulate starting composition may be prepared by any suitable tower or non-tower method, such as spray drying or dry mixing. If desired, the particulate starting material may be prepared by mixing at least a portion in the high speed mixer / granulator itself. The particulate starting material may consist at least in part of a spray dried powder.

The final granular material has a bulk density of at least 650 g / liter, preferably at least 700 g / liter. It is characterized by a particularly low particle porosity, preferably not more than 0.25, more preferably not more than 0.20, which allows it to be distinguished even from the highest density powders made by spray drying alone.

The final granular material may be used as such in a complete detergent composition. Alternatively, it may be mixed with other components or mixtures prepared separately and may form the majority or the minority of the final product. In general, any additional ingredients such as enzymes, bleaches and fragrances that are not suitable for performing the granulation process may be mixed with the granular material to form the final product.

For example, in one embodiment of the present invention, a detergent base powder is prepared by spray drying an aqueous slurry of heat incompatible and compatible ingredients. If desired, other ingredients may then be mixed.
The resulting powder is densified and granulated to form the product of this invention. Still other ingredients may optionally be mixed after granulation. The densified granular material of the present invention may typically comprise 40-100% by weight of the final product.

In another embodiment of the invention, one or more biomaterials and / or one or more premixes of biomaterials are dried in the high speed mixer / granulator itself or in another device. Mix to prepare a detergent base powder, which is then densified and granulated to form the final product of the invention. Furthermore, if desired, further ingredients may be added after granulation.

In yet another embodiment of the present invention, the granular material prepared according to the present invention is an "adduct" containing a relatively high level of detergent actives on an inorganic carrier, which is mixed with a small amount of other ingredients. May be mixed with to form the final product.

Method In the method of the present invention, the granular starting material (detergent base powder) prepared by any suitable method is mixed in a high speed mixer /
Granulate in a granulator to increase its bulk density,
At the same time it improves its powder properties. The method of the present invention has excellent washing performance and is a route for producing a very dense granular detergent composition containing low to moderate levels of anionic surfactant and high levels of aluminosilicate forming agent. I will provide a.

Preferred starting powders are: (a) at least partly composed of anionic detergent actives
It consists of 17 to 35% by weight of non-soap detergent active substance, and (b) 28 to 45% by weight of crystalline or amorphous sodium aluminosilicate, the weight ratio of (b) :( a) is 0.
9: 1 to 2.6: 1, 100% with optional addition of other detergent ingredients
Weight%

For treatment in a high speed mixer / granulator by the method of the present invention, this produces a granular detergent composition or ingredient according to the first aspect of the present invention. However, the method of the invention also yields good results with compositions containing low levels of detergent actives.

In the method of the present invention, granulation is performed using a high speed mixer / granulator having a stirring function and a cutting function. Preferably, the stirrer and the cutter may be operated independently and independently of each other at adjustable speeds. Such mixers can combine high energy agitation input with cutting capability, but can be used to provide other gentle agitation regimes, whether or not a cutter is used during operation. is there. Thus it is part of a very versatile and easy to control device.

A preferred type of high speed mixer / granulator for use in the method of the present invention is a bowl type, preferably with a substantially vertical stirring axis. Fukal of Japan is especially preferable
Fukae (registered trademark) FS-G series mixer manufactured by Powtech Kogyo Co. The device is essentially in the form of a pot-shaped container that can be moved in and out of the top door, with a stirrer having a substantially vertical axis near its bottom, with a cutter on the side wall. The stirrer and the cutter may be operated independently of each other and separately at adjustable speeds.

Other similar mixers found to be suitable for use in the method of the present invention are Dierks & Sohne Dio, West Germany.
sna (registered trademark) V series and UK TK Field Ltd.
Pharma Matrix (registered trademark). Other similar mixers believed suitable for use in the method of the present invention include Fuji Sangyo Co.'s Fuji® VG-C series and Italian Zanchetta & Co srl's Roto ( Registered trademark).

Another mixer found suitable for use in the method of the present invention is Morton Machi, Scotland.
It is a mixer of the Lodige (registered trademark) FM series group manufactured by ne Co. Ltd. It differs from the above mixer in that the stirrer has a horizontal axis.

As mentioned above, in order to perform granulation and densification, it is essential to use a high speed mixer / granulator in the method of the present invention. If desired, the mixer may also be used in a pretreatment step before carrying out the granulation.

For example, it is within the scope of the invention to prepare the particulate starting material by mixing, at least in part, in a high speed mixer / granulator. Therefore,
The dry mixed starting material may be prepared from the raw material in a high speed mixer / granulator, or other premixed powders in which one or more additional ingredients are prepared in another way (eg by spray drying). May be mixed with. A suitable agitation / cutting regime and residence time may be selected depending on the materials to be mixed.

Another pretreatment that can be performed in a high speed mixer / granulator is micronization. In any case, this is necessary, among other things, depending on the method of preparation of the starting powder and its water content. For example, powders prepared by spray-drying may require more micronization than powders prepared by dry mixing. In addition, the appropriate agitation / cutting regime can be selected due to the ease of control of the device. Generally, the speeds of the stirrer and the cutter are relatively high. Relatively short residence times (eg 2-4 minutes for a 35 kg batch) are generally sufficient.

An essential feature of the process of the invention is the granulation stage, during which time there is a very high degree of densification of at least 650 g / l, preferably at least 700 g / l, with a very uniform particle size and general It produces a high density granular material in the form of spherical particles.

Granulation is performed by operating the mixer at a relatively high speed using a stirrer and a cutter. Relatively short residence times (eg 5-8 hours for a 35 kg batch) are generally sufficient. The final bulk density can be controlled by the choice of residence time, but if the bulk density cannot be increased to at least 650 g / liter, the powder properties of the resulting granular material are not optimal.

The presence of a liquid molding agent is a prerequisite for successful granulation. Since higher levels can result in poor flow properties of the final granular material, the amount of additive molding agent preferably exceeds that required to bring the anhydrous content of the composition to greater than about 6% by weight. Absent. If necessary, a molding agent,
Water may preferably be added before or during granulation, but some starting powders may inherently contain a sufficient amount of water. If a liquid molding agent is to be added, it may be sprayed on during the mixer operation.

In one preferred mode of operation, the mixer is first operated at a relatively low speed during the addition of the molding agent and then the mixer speed is increased to effect granulation.

If the starting material has a sufficient water content and it is not necessary to add a molding agent, then micronization (if necessary) and granulation should be considered as a single operation rather than as separate process steps. In fact, in that case, whether or not micronization is necessary, it is not necessary to predetermine. Since the mixer conditions required are generally substantially the same as those required for micronization and granulation, the mixer need only do the necessary things.

According to a preferred embodiment of the invention, granulation is carried out at a controlled temperature somewhat above ambient temperature, preferably above 30 ° C. The optimum temperature is obviously formulation dependent, but in general
It is in the range of 30-45 ° C, preferably about 35 ° C.

It is an indispensable feature of the present invention that, like the above-mentioned Japanese Patent No. 61 069897 A (Kao), the "agent for improving surface characteristics" is not contained during granulation. When processing formulations with a relatively high ratio of aluminosilicate forming agent to surfactant,
According to the present invention, it is not only unnecessary to use finely divided powdery substances such as finely divided sodium aluminosilicate during the granulation stage, but which formulation makes granulation more difficult? Or even make it impossible.

Optional Flow Aids According to a preferred embodiment of the present invention, finely ground granular flow aids may be mixed with the granular material after granulation is complete. The flow aid is conveniently added while the granular material is still in the high speed mixer / granulator, and the low speed mixer is run for an additional short period of time. No further granulation occurs at this stage. It is also within the scope of the invention to transfer the granulate to a different device and then add the flow aid to it. This embodiment of the present invention provides the above Japanese Patent No. 61 06989 in which a "surface property improving agent", which may be finely divided sodium aluminosilicate, is included during the granulation step itself.
It needs to be distinguished from the conventional technical process of 7A (Kao). It is within the scope of the invention to add a particulate flow aid after granulation is complete, however, as noted above, it is essential to the invention that the finely crushed particulate material "surface property modifier" is not included during granulation. Is. The addition of flow aids after the completion of granulation has an additional beneficial effect on the properties of the granular material regardless of formulation, while the presence of this kind of material during the granulation step in the process of the invention Processing becomes more difficult.

During the subsequent flow aid mixing, the preferred granulation temperature is 30
It may be maintained at ~ 45 ° C, preferably about 35 ° C.

This flow aid is a finely crushed granular material. The preferred average particle size is 0.1 to 20 microns, more preferably 1 to 10 microns.

According to one preferred embodiment of the present invention, the flow aid is a finely crushed amorphous sodium aluminosilicate, as described and claimed in our specification (Japanese Patent Application No. 1-111944) filed concurrently on the same date. Is. A suitable material is the registered trademark Alusil of Warsington, Cheshire, England.
Commercially available from Crosfield Chemicals Ltd. This material is effective at improving flow properties even at very low levels and has the effect of increasing bulk density. Therefore,
The bulk density can be adjusted by appropriately selecting the level of amorphous sodium aluminosilicate added after granulation.

0.2 to 5.0% by weight, more preferably 0.5 to 3.0% by weight, based on the starting powder, of amorphous sodium aluminosilicate
To use effectively.

Another preferred flow aid is finely ground crystalline sodium aluminosilicate. The crystalline aluminosilicates conventionally considered in connection with molding agents are also suitable for use as flow aids. However, they have lower weight-potency values than amorphous substances and are suitably used in amounts of 3.0 to 12.0% by weight, preferably 4.0 to 10.0% by weight.

If desired, crystalline sodium aluminosilicate and amorphous sodium aluminosilicate may be used simultaneously or subsequently as flow aids.

Alternative flow aids suitable for use in the method of the present invention include precipitated silicas such as Neosyl® and precipitated calcium silicates such as Microcal®, both of which are available in Crosfield. Commercially available from Chemicals Ltd. (Warrington, Cheshire, UK).

The invention is illustrated in more detail by the following non-limiting examples, in which parts and percentages used are expressed by weight, unless stated otherwise.

Examples Example 1 A detergent composition was prepared by spray-drying an aqueous slurry so that the water content was substantially zero, with the following composition: parts linear alkyl benzene sulfonate 24.0 nonionic surfactant 2.0 soap 1.0 Zeolite (anhydrous) 38.0 Water combined with zeolite 10.84 Sodium silicate 4.0 Acrylate / malate copolymer 2.0 Minor components 2.0 Sodium carbonate 10.0 94.64 The ratio of zeolite (anhydrous) to non-soap surfactant in this composition was 1.46. Please note that.

35 kg of this spray-dried powder was introduced into a Fukae® FS-G series high speed mixer / granulator for 2-4
Micronized at high speed for a minute. Water (2.0 parts) was then sprayed on while the mixer was running at low speed, then speeded up for 5-8 minutes while maintaining the temperature at about 35 ° C. Granulation occurred during this period.

A sample of granular product was removed from the mixer. It was free flowing and showed no tendency to cake. Its dynamic flow rate was 65 ml / sec.

Alcyl Al, a fine amorphous sodium aluminosilicate
The usil 1.0 part was introduced into the Fukae mixer and then the mixer was run at low speed for 1 minute. The resulting granular product was free flowing and showed no tendency to cake. Its bulk density is 740 g / liter,
Its particle porosity was less than 0.20. Its average particle size was 405 microns and its dynamic flow rate was 105 ml / sec.

The following ingredients were then mixed with the granular material to produce 99 parts of final detergent powder: Colored granules 1.5 parts Enzyme (Alcalase) 0.61 parts Perfume 0.25 parts Examples 2 and 3 Spray dried powder used in Example 1 20 kg was introduced into the Fukae® FS-30 high speed mixer / granulator,
Micronized for 4 minutes. Then water (0.8 kg) was added and the mixture was granulated for 4 minutes while maintaining the temperature at about 35 ° C. Remove the specimen (Example 2) from the mixer,
Its powder properties were determined: these are shown in Table 1 below.

The finely ground amorphous sodium aluminosilicate, Arsil® (0.2 kg) was then added. The physical properties of the resulting powder (Example 3) are shown in Table 1 below, which shows the effect on flow and bulk density when a flow aid is added after granulation is complete. The beneficial effect is obvious. The inclusion of arsyl increases the content of fine particles <180 microns, but not to acceptable levels.

Comparative Example A 20 kg of the spray dried powder used in Example 1 was introduced into a Fukae high speed mixer / granulator and pulverized for 4 minutes. The finely ground amorphous sodium aluminosilicate, Arsil® (0.2 kg), was then introduced into the mixer. Then water (0.8 kg) was added and the mixture was granulated for 4 minutes while maintaining the temperature at about 35 ° C.
The physical properties of the resulting powder are shown in Table 1 below, which shows the detrimental effect of adding arsyl prior to granulation. Note that the increase in fines content is significantly greater than the addition of arsyl prior to granulation.

Comparative Example B This comparative example describes an attempt to carry out the process of the invention with different spray-drying formulations containing high levels of anionic surfactant and relatively low levels of sodium aluminosilicate. The formulation is as follows: parts spray dried base linear alkyl benzene sulfonate 26.0 sulfuric acid primary alcohol 8.0 nonionic surfactant 1.0 soap 3.0 zeolite (anhydrous) 14.8 zeolite bound water 4.2 sodium silicate 6.0 sodium carbonate (light soda ash ) 5.0 Sodium sulphate 4.0 Acrylate / maleate copolymer 1.0 Moisture 4.0 Post-added zeolite (hydrate) ^* 5.0 Sodium carbonate (granular) 15.0 Nonionic surfactant 3.0 100.0 ^* 3.9 parts equivalent to anhydrous zeolite Zeolite (anhydrous) ) To non-soap surfactant (0.53) was less than 0.9: 1.

Place the spray-dried base powder (7.7 kg) in a Geosna Diosna® high speed mixer / granulator for 5.0
Parts (0.3 kg) of nonionic surfactant were sprayed on and 15 parts of granular soda ash (1.5 kg) and 5 parts of zeolite (0.5 kg) were added. An attempt was made to micronize for 1 minute at a stirrer speed of 196 rpm and a cutter speed of 3000 rpm, but the mixture was overgranulated into large lumps and overheated.

Examples 4 and 5 35 kg of the spray-dried powder used in Example 1 were introduced into a Regige Lodige® FM series high speed mixer / granulator and pulverized for 4 minutes. The mixer was then sprayed with water (1.1 kg, 35%) while the mixer was running at the same speed and then the mixer was run for an additional 3 minutes while maintaining the temperature at about 35 ° C. Granulation occurred during this period. The sample (Example 4) was removed from the mixer and its powder properties were determined:
These are shown in Table 2 below.

The finely ground amorphous sodium aluminosilicate, Arsil® (1.2 kg) was then introduced into the mixer and they were run for an additional 5 minutes. The physical properties of the resulting powder (Example 3) are shown in Table 2 below. The results were similar to those obtained in Examples 2 and 3 using a Fukae mixer.

Comparative Example C 28.8 kg of the spray-dried powder used in Example 1 was introduced into a Regige® FM series high speed mixer / granulator and pulverized for 4 minutes. The finely ground amorphous sodium aluminosilicate, Arsil® (1.2 kg) was then introduced into the mixer. While continuing to operate the mixer, spray water (1.1 kg, 3.5%), then raise the temperature to about 35
The mixer was run for an additional 3 minutes while maintaining the temperature at 0 ° C. Granulation occurred during this period. The physical properties of the resulting powder are shown in Table 2 below.

COMPARATIVE EXAMPLE D Using the spray-dried formulation similar to that used in Comparative Example B, containing a high level of anionic surfactant and a relatively low level of sodium aluminosilicate, Regige Lodige.
An attempt to carry out the process of the invention in a mixer is described in this comparative example. The formulation is as follows: Parts Linear alkyl benzene sulfonate 26.0 Sulfuric acid primary alcohol 8.0 Nonionic surfactant 1.0 Soap 3.0 Zeolite (anhydrous) 10.9 Zeolite bound water 3.1 Sodium silicate 6.0 Sodium carbonate 5.0 Sodium sulfate 4.0 Acrylate / malate Copolymer 1.0 Moisture 2.9 68.9 The ratio of zeolite to non-soap surfactant (0.31) is 0.9: 1.
Was less than.

The formulation material (30 kg) was placed in a Regige FM mixer and the mixer was run for 4 minutes as in Examples 4 and 5 and Comparative Example C. No dusty finely crushed powder was obtained and it was not clear if pulverization had occurred. Then, water (1.05 kg, 3.5%) was added in the same manner as in the above example, and granulation was tried for 0.5 minutes, but the result was doubtful.

Examples 6 to 8 The indicator composition shown in Example 1 was spray dried to three different moisture contents, 3 as shown in Table 3 below.
Different types of powder were prepared. Since 38.0 parts of zeolite (anhydrous main component) in the formulation requires 10.84 parts of water for hydration,
The water content of each powder is obtained by subtracting the numerical value from the total water content. Note that the powder of Example 6 was overdried, while the powder of Example 8 contained 3.16 parts moisture.

A 10 kg batch of each powder was placed in a Geosna® V series mixer with a stirrer speed of 196 rpm and a cutter speed of 3000.
Granulated (and micronized if necessary) at rpm. In the case of Examples 6 and 7, where the first micronization occurs, water was sprayed into the mixer in the indicated amount and time before granulation. After the granulation was complete, finely crushed amorphous sodium aluminosilicate arsyl (0.1 kg) was mixed into the granular material. The properties of the three types of granular material are shown in Table 3.

Example 9 This example describes a method of adding an additional component (sodium carbonate) to the spray-dried base powder in a mixer prior to micronization and granulation. The formulation is as follows: parts spray dried base linear alkyl benzene sulfonate 24.0 nonionic surfactant 2.0 soap 1.0 zeolite (anhydrous) 38.0 zeolite bound water 10.84 sodium silicate 4.0 acrylate / maleate copolymer 2.0 minor component 2.0 84.04 Sodium carbonate added in the mixer 10.0 94.04 8.5 kg of spray-dried basic powder and 1.0 kg of sodium carbonate (light soda ash) were placed in a Diosna V100 mixer and atomized for 4 minutes at a stirrer speed of 196 rpm and a cutting machine speed of 3000 rpm. Water (0.45 kg) was added over 2 minutes while the mixer was operating at a stirrer speed of 98 rpm and a cutter speed of 1500 rpm, and then the admixture was granulated for 5 minutes at a stirrer speed of 196 rpm and a cutter speed of 3000 rpm.

Finally, the agitator speed was 98 rpm and the cutter was switched off to mix the arsir (0.1 kg) while running the mixer.

The properties of the resulting granular material are as follows: bulk density (g / liter) 780 dynamic flow rate (ml / sec) 133 compressibility (% v / v) 7 particle size (micron) 839 particles The ratio of aluminosilicate to non-soap surfactant in the granulated mixture with a porosity of 0.10 was 1.46.

Example 10 This example describes a method in which an anionic surfactant is partly passed through a spray-dried base powder and partly added to the base powder, introduced into a mixer, and then pulverized and granulated. Enter. The prescription is as follows.

Parts Spray-dried base Linear alkyl benzene sulfonate 12.0 Nonionic surfactant 2.0 Soap 1.0 Zeolite (anhydrous) 38.0 Zeolite bound water 10.84 Sodium carbonate (light soda ash) 10.0 Sodium silicate 4.0 Acrylate / malate copolymer 2.0 Minor components 2.0 81.84 Mixer put the additive linear alkyl benzene sulphonate (powder) 12.0 93.84 spray-dried basic powders 16.5kg and linear alkyl benzene sulphonate powder (Marlon Marlon (registered trademark) A390 Huls Co.) 2.4 kg in Jiosuna V100 mixers, agitator speed 196rpm And pulverized at a cutter speed of 3000 rpm for 4 minutes.
The mixer is agitator speed 98 rpm and cutting machine speed 1500 rpm.
Add water (0.45 kg) over 2 minutes while operating at
The mixture is then stirred at a stirrer speed of 196 rpm and a cutter speed of
Granulate for 5 minutes at 3000 rpm. During the granulation period, the temperature should be 40
Raised to ℃. Finally, with the agitator speed at 98 rpm and the mixer switched off, run the arsir (0.
19 kg) were mixed.

The resulting granular material had the following properties: bulk density (g / liter) 714 dynamic flow rate (ml / sec) 55 compressibility (% v / v) 17 particle size (micron) 712 Particle porosity <0.20 The ratio of aluminosilicate to non-soap surfactant in the granulated mixture was 1.46.

Examples 11 and 12 These examples include a method of densifying and granulating powders prepared by dry mixing in a high speed mixer / granulator. Prepare the following formulation materials by mixing in a concrete mixer: Part Linear alkyl benzene sulfonate 24.0 Nonionic surfactant 2.0 Soap 1.0 Zeolite (anhydrous) 38.0 Zeolite bound water 10.84 Sodium carbonate (light soda ash) 10.0 Sodium silicate 4.0 Acrylate / malate copolymer 2.0 Minor components 2.0 92.24 The ratio of aluminosilicate to non-soap surfactant in this mixture was 1.46.

20 kg of the formulated material 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.
The mixer is agitator speed 98 rpm and cutting machine speed 1500 rpm.
Add water (0.2 kg) over 2 minutes while operating at
The mixture is then stirred at a stirrer speed of 196 rpm and a cutter speed of
Granulate for 4 minutes at 3000 rpm. A sample (Example 11) was taken and its powder properties were measured (see below). Finally, mix the arsir (0.2 kg) while operating the mixer with the agitator speed 98 rpm and the cutter switched off,
The powder properties of the final granular material (Example 12) were also measured.

The powder properties of the granular material before and after addition of arsyl were as follows: 11 12 Bulk density (g / l) 780 810 Dynamic flow rate (ml / sec) 80 96 Compressibility (% v / v) ) 17.0 15.3 Particle size (microns) -607 Particle porosity <0.20 <0.20 Example 13 Fuukae FS-1200 mixer was used to prepare the following formulation materials by the dry mix method: premix parts linear alkylbenzene sulfonate ^* 25.0 Stone 1.0 Zeolite (hydrate) ^** 35.0 Sodium carbonate (light soda ash) 15.51 Sodium silicate 4.0 Acrylate / malate copolymer 1.0 Minor component 3.88 ^* Mallon A390 powder (90% activity: indicated number is 100 %
^* 27.3 Parts of anhydrous zeolite added into the mixer in the same amount Nonionic surfactant 2.0 Water 1.5 Post-added zeolite (hydrate) 10.0 97.39 Ingredients described in "Premix", Mix for 2 minutes at a stirrer speed of 80 rpm and a cutter speed of 2000 rpm in a fluff mixer. The nonionic surfactant was then added over 1 minute, followed by water over 2 minutes while the mixer was running at the same stirrer speed and cutter speed. Then granulate at the same speed for 6 minutes and finally still add the zeolite at the same speed for 2 minutes.

The properties of the resulting granular material were as follows: bulk density (g / liter) 780 dynamic fluidity (ml / sec) 83 compressibility (% v / v) 11.8 particle size (micron) 477 Particle Porosity 0.1 The ratio of zeolite (anhydrous) to non-soap detergent active in the granulated material was 1.0.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Michael William Hollingsworth England, Merseyside, Willal, Bebington, Davins Hay 129 (72) Inventor Keiichi Kawabuchi 4-19 Nishiogita, Suginami-ku, Tokyo ―4 (72) Inventor Donald Peter England, Wilal, Thornton Hook, Eaton Drive ・ 74 (72) Inventor Peter Zyon Rutsel 265-2 Yamate-cho, Naka-ku, Yokohama-shi, Kanagawa (56) Reference Document JP-A-62-236897 (JP, A)

Claims (10)

[Claims] 1. A bulk density of at least 650 g / liter,
And a granular detergent composition having a particle porosity of less than 0.25 or a component therefor, comprising: (a) 17-35% by weight of a non-soap cleaning active substance, at least part of which comprises an anionic cleaning active substance. And (b) containing 28 to 45 weight percent (anhydrous basis) of crystalline or amorphous sodium aluminosilicate,
The above composition, wherein the weight ratio of (b) :( a) is from 0.9: 1 to 2.6: 1 and is 100% by weight with the addition of any other detergent component. 2. A composition according to claim 1 having a bulk density of at least 700 g / liter and a particle porosity of less than 0.20. 3. The composition according to claim 1, wherein the weight ratio of (b) :( a) is 1.2: 1 to 1.8: 1. 4. A method for producing a granular detergent composition or component having a bulk density of at least 650 g / liter and a particle porosity of less than 0.25, wherein (a) at least a portion of the anionic detersive active substance is used. 5 to 35% by weight of a non-soap cleaning active substance, and (b) 28 to 45% by weight (anhydrous basis) of crystalline or amorphous sodium aluminosilicate, (b): (a)
In a high-speed mixer / granulator having a stirring function and a cutting function, in which a granular starting material having a weight ratio of at least 0.9: 1 and any other cleaning component added so as to be 100% by weight is added. , In the presence of a liquid binder, without the presence of finely divided granular surface property modifiers, whereby granulating and densifying to a bulk density of at least 650 g / l. The method characterized by the above. 5. The method according to claim 4, wherein the bulk density is at least 700 g / liter and the particle porosity is less than 0.20. 6. The method according to claim 4, wherein the amount of the non-soap cleaning active substance is 17 to 35% by weight. 7. The method according to claim 4 or 5, wherein the weight ratio of (b) :( a) is 0.9: 1 to 2.6: 1. 8. A method according to any one of claims 4 to 7 in which the granulation is carried out in a bowl type high speed mixer / granulator having a substantially vertical stirring shaft. 9. A process as claimed in any one of claims 4 to 7 in which the particulate starting material consists at least in part of a spray dried powder. 10. A method according to claim 4 wherein the particulate starting material is prepared, at least in part, by mixing in a high speed mixer / granulator followed by granulation.
7. The method according to any of items 7.