JPH01318097A - Detergent composition and production thereof - Google Patents

Abstract

PURPOSE: To provide a granular detergent having excellent washing performance, powder characteristic and a high bulk density, by performing a specified granulating and condensation to the starting material, to which non-soap washing active material, which includes anion washing active material, and sodium aluminosilicate are added.

CONSTITUTION: At the time of manufacturing the granular detergent composition or component having a bulk density, at least, at 650g/l and grain porosity less than 0.25, granular starting material, which includes (a) non-soap washing active material, of which one part is formed of anion washing active material, at 5-35wt.%, (b) crystal or non-crystal sodium aluminosilicate at 28-45wt.% (anhydride reference) so that weight ratio of (a):(b) is set at 0.9:1 and to which desirable other detergent component is added so that weight ratio satisfies 100wt.%, is processed in a high speed mixer/granular having an agitating function and a cutting function under the existence of the liquid binder without existence of a granular surface characteristic improving agent, which is finely divided.

COPYRIGHT: (C)1989,JPO

Description

DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a high bulk density granular detergent composition having good washing performance and good powder properties, and to a process for producing the same.

BACKGROUND AND PRIOR ART In recent years, within the detergent industry, relatively high
There has been considerable interest in producing detergent powders with bulk densities of g/liter and higher. Particular attention is paid to the densification of the spray-dried powder by post-treatment. European Patent No. 219328A (Unllever) teaches spray-drying a slurry to produce a base powder containing low to moderate levels of sodium tripolyphosphate extruding agent and low levels of inorganic salts, and then drying at a high bulk density. and by post-adding a solid material containing sodium sulfate with a particle size smaller than that of the base powder, thus filling the cavities between the base powder particles and producing a product of high bulk density. A detergent composition is shown. 1988
European Patent No. 270240A issued on June 8,
Unllever) has a particle porosity of less than 0.40 and contains anionic surfactants, optional nonionic surfactants, aluminosilicate molding agents, polymeric polycarboxylates, and preferably sodium carbonate. Spray-dried phosphorus-free base powders containing low or zero levels of electrolytes are 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.

European Patent No. 229671A (Kao) shows the post-addition of crystalline alkaline inorganic salts, such as sodium carbonate, to spray-dried powders to produce high bulk density products.

West German Patent No. 1517713 (Un1lever)
describes a different approach in which detergent powders produced by spray drying or pan granulation are spheronized and granulated in a "Marmerizer"® to increase the bulk density somewhat. There is.

Japanese Patent No. 610Ei9897 A (Kao)
Spray-dried detergent powders containing surfactants and shaping agents were successfully milled and granulated in a high speed mixer/granisator, the granulation being carried out in the presence of a "surface property modifying agent" and optionally a shaping agent. It shows how to do it. In the high speed mixer/granulator, the spray-dried powder would first be crushed and broken down into a fine powder. Surface modifiers and optional forming agents are then added and the finely divided material is granulated to form a high bulk density final product.

A finely divided particulate solid, such as finely divided sodium aluminosilicate, is clearly necessary to prevent clumping of the ball or cake-sized composition. Examples of spray-dried starting powders described in the Kao specification include very high levels of surfactants (45% by weight) and relatively low levels of forming agent salts, which are cake-like. It is thought that it is very easy to form into a ball shape.

European Patent No. 220024 A (Procter&
Gamble) is also associated with densification of spray-dried powders containing high levels (30-85% by weight) of anionic surfactants. The powder is consolidated and granulated, but before consolidation an inorganic shaping agent (sodium tripolyphosphate or sodium aluminosilicate and sodium carbonate) is added.

If the final powder is precisely formulated, especially with respect to the amount of surfactant and the ratio of surfactant to containing extrusion agent, it is possible to avoid the use of "surface-modifying agents" or similar finely divided substances.
The inventors have now discovered that high bulk density detergent compositions can be produced by granulating the spray-dried powder or dry blended powder in a high-speed mixer/granulator after micronization, if desired.

Definition of the Invention Firstly, the present invention provides: 1 having a bulk density of at least 650 g/liter and (a) consisting at least in part of an anionic detergent active substance;
7-35% by weight of non-B soap detergent actives, and (b)
28-45% by weight (anhydrous main component) of crystalline or amorphous sodium aluminosilicate, (b) vs. (a)
The weight ratio of 0.9+1 to 2. lli: 1, preferably 1.2: 1 to 1.8: 1, 100% by weight
To provide a granular detergent composition to which other detergent ingredients are optionally added so as to achieve the following.

Secondly, the present invention provides a method for making a granular detergent composition or ingredient having a bulk density of at least 650 g/liter, which method comprises: (a) consisting at least in part of an anionic detergent active; ~35% by weight of a non-B soap detergent active, and (b) 28-45% by weight (anhydrous main component) of crystalline or amorphous sodium aluminosilicate, wherein the weight ratio of (b) to (a) is At least 0.9:
1, optionally adding other detergent ingredients to 100% by weight
A granular starting material consisting of a granular starting material of by at least 650
It consists of granulation and densification to a bulk density of g/l.

DETAILED DESCRIPTION OF THE INVENTION Product A first aspect of the invention is a dense granular detergent powder that combines high bulk density, good surface properties and excellent cleaning and laundering performance, which is also the subject of the invention. It can be easily and conveniently manufactured by certain methods.

The detergent compositions of the present invention are characterized by their combination of excellent properties and easy processability for a moderate content of surfactants that are at least partially anionic and relatively high levels of sodium aluminosilicate shaping agents. I owe it to you. If the absolute amounts of powdered aluminosilicate molding agent and surfactant and their mutual ratios are selected appropriately, they may be added during the granulation step as prescribed in Japanese Patent No. 81069897A (Kao). The inventors have discovered that the powder may be granulated in a high speed mixer/granulator without the need to use "surface property modifying agents". The resulting dense granules exhibit good flow properties and are comparable, at least in terms of cleaning and laundering performance and cold water dispersion ability, to compositions described in Kao's specification containing substantially higher levels of surfactants. be.

The aluminosilicate molding agents present in the compositions of the present invention may be crystalline or amorphous or mixtures thereof, and these materials contain some bound water. , it is necessary to have a calcium ion exchange capacity of at least about 50 mg CaO/g. Preferred aluminosilicates have 1.5 to 3.5 S i O units (in the above two formulas)
containing about 100 microns or less, preferably 20
Particle size is submicron.

As described in detail in the literature, amorphous and crystalline aluminosilicates can be easily made by the reaction between sodium silicate and sodium aluminate.

In the present invention, crystalline aluminosilicate (zeolite)
It is preferable to use For example, West German Patent No. 147320
Suitable materials are described in German Patent No. 1 (Henkel) and German Patent No. 1 429 143 (Procter & Gamble). Preferred sodium aluminosilicates of this type are the well-known commercial zeolites A and X and mixtures thereof. Particularly preferred for use in the present invention is type 4A zeolite.

Aluminosilicate molding agent (anhydrous main component) in the composition of the present invention
The ratio of total non-toxic surfactants is preferably 1.2+
1-1.11: Within the range of 1.

The non-B surfactant contained consists at least in part of an anionic surfactant. It may be well known that suitable anionic surfactants require special techniques; examples thereof include linear alkylbenzene sulfonates, especially those having alkyl chains of length C to C15. Straight-chain sodium alkylbenzene sulfonates; secondary and secondary alkyl sulfates, especially 012-C15-secondary alcohol sodium sulfates; sulfuric acid alkyl ethers; alpha olefin sulfonates and internal olefin sulfonates;
Alkanesulfonate; dialkyl sulfosuccinate;
fatty acid ester sulfonates; and combinations thereof.

If desired, the starting powder may contain preferably small amounts of nonionic surfactants. It is believed to be well known that nonionic surfactants also require special techniques, but -alcohol ethoxylates, especially CI2-C, which are ethoxylated with an average of 3 to 20 moles of ethylene oxide per mole of alcohol. Primary alcohols and C12-C15 secondary alcohols are mentioned.

The surfactant component of the composition of the present invention may suitably be comprised of 10-35% by weight anionic surfactant and 0-10% by weight nonionic surfactant.

Other types of non-climate surfactants may optionally be included, such as cationic surfactants, zwitterionic surfactants, amphoteric surfactants or semipolar surfactants. A large number of suitable detergent-active compounds are available, which are described in the literature, for example in "Surfactants and Detergents J" (Schwartz,
Co-authored by Perry and Berc, Volumes 1 and 2
(Volume).

Optionally, soap may be included to provide suds control and additional cleaning power as well as molding agent powder. A total surfactant content of 17-35% of the composition of the invention does not contain soap.

The compositions of the present invention preferably contain no more than 5% by weight of phosphate formers, and more preferably are substantially free of phosphate formers.

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

The particulate starting material may consist at least in part of a spray-dried powder.

The final granulate has a bulk density of at least 650 g/l, preferably at least 700 g/l. It has a particularly low particle porosity, preferably 0.2
It is characterized by a porosity of not more than 5, more preferably not more than 0.20, which allows it to be distinguished even from the densest powders made only by spray drying.

The final granulate may be used as a complete detergent composition as such. Alternatively, it may be mixed with other components or mixtures prepared separately and may form a major or minor portion of the final product. In general, any additional ingredients such as enzymes, bleaching agents, and fragrances that are not suitable for granulation processing may be mixed with the granulated material to form the final product.

For example, in some embodiments of the invention, heat refractory and +! 4
Wash by spray drying the aqueous slurry solution of the soluble ingredients.
Prepare the base powder. Other ingredients may then be mixed in, if desired. The resulting powder is densified and granulated to form the product of the invention.

Further other ingredients may be mixed in after granulation, if desired. The densified granular material of the present invention may typically constitute 40-100% by weight of the final product.

In another embodiment of the invention, the one or more biological substances and/or one or more brimixes of biological substances are dry mixed in the high speed mixer/granulator itself or in other equipment. to prepare a detergent base powder, which is then densified and granulated to form the final product of the present invention. Furthermore, additional components may be added after granulation if desired.

In yet another embodiment of the invention, the granular material prepared according to the invention is an "adduct" containing relatively high levels of detergent actives on an inorganic carrier, with small amounts of other ingredients. may be mixed with to form the final product.

Method In the method of the 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 provides a route for the production of very dense granular detergent compositions containing low to moderate levels of anionic surfactants and high levels of aluminosilicate shaping agents, with excellent wash performance. I will provide a.

Preferred starting powders consist of (a) 17 to 35% by weight non-carrier detergent active, consisting at least in part of anionic detergent active, and (b) 28 to 45% by weight crystalline or amorphous sodium aluminosilicate. The weight ratio of (b):(a) is 0.9:1 to 2.6:1, and other detergent components are optionally added to make up to 100% by weight.

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

In the method of the present invention, granulation is carried out using a high speed mixer/granulator having stirring and cutting functions. Preferably, the stirrer and cutter may be operated independently of each other and at separately adjustable speeds. Such mixers are capable of combining high-energy agitation input with cutting functionality, but can also be used to provide other gentle agitation regimes, with or without a cutting machine during operation. be. It is thus a piece of equipment that is very versatile and easy to control.

The preferred type of high speed mixer/granulator for use in the process of the invention is bowl-shaped and preferably has a substantially vertical stirring shaft. Particularly preferable is Japanese F u
kal Powtech K ogyo C.

This is a mixer from the Fukae (registered trademark) FS-C series manufactured by Fukae Corporation. This device is essentially in the form of a pot-shaped container that can be accessed through an upper doorway, with a stirrer having a substantially vertical axis near its bottom and a cutting device in the side wall. The stirrer and cutter may be operated independently of each other and at separately adjustable speeds.

Other similar mixers found suitable for use in the method of the invention include D Ierks & S.
D 1osna (registered trademark) V series manufactured by Ohne and P manufactured by TKF 1eld Ltd., UK.
harlIa Matrix (registered trademark). Other similar mixers believed to be suitable for use in the method of the invention include F ujj S ang of Japan;
YO Co., Inc., Fujil (registered quantity [) VC-C series) and Roto (registered trademark), manufactured by Z anchetta & Co5r1 in Italy.

Another mixer that has been found suitable for use in the method of the invention is the Morton mixer from Scotland.
Machine Co, Ltd.
(registered trademark) is a mixer in the FM series group. This differs from the mixer described above in that the stirrer has a horizontal axis.

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

For example, as noted above, it is within the scope of the present invention to prepare particulate starting materials at least in part by mixing in a high speed mixer/granulator. therefore,
A dry mixed starting material may be prepared from the biological material in a high speed mixer/granulator or one or more further ingredients may be prepared in another way (e.g. by spray drying) with other premixed powders. May be mixed. Appropriate stirring/cutting regimes and residence times may be selected depending on the materials being mixed.

Another pretreatment that can be carried out in a high speed mixer/granulator is micronization. In any case, this is necessary depending on, among other things, 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 blending. Furthermore, the equipment is easy to control so that an appropriate stirring/cutting regime can be selected. Generally speaking, stirrers and cutters are faster than TRT. Relatively short residence time (
eg 2-4 minutes for a 35 kg batch) is generally sufficient.

An essential performance of the process of the invention is the granulation stage, during which densification takes place to a very high value of at least 650 g/l, preferably at least 700 g/l, and the particle size is very uniform and common. produces dense granular material in the form of spherical particles.

Granulation is carried out by operating the mixer at relatively high speeds using an agitator 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 unless the bulk density can be increased to at least 650 g/l, the powder properties of the resulting granulate material will not be optimal.

The presence of a liquid forming agent is a prerequisite for successful granulation. The amount of added shaping agent preferably exceeds the amount necessary to achieve an anhydrous content of the composition greater than about 6% by weight, as high levels can result in deterioration of the flow properties of the final granulate. do not have. If necessary, molding agent,
Water may preferably be added before or during granulation, but some starting powders inherently contain sufficient amounts of water. If a liquid forming agent is to be added, it may be sprayed during mixer operation.

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

If the starting material has a sufficient water content so that there is no need to add shaping agents, micronization (if necessary) and granulation should not be considered as separate process steps, but as tll-operations. In fact, there is no need to predetermine whether micronization is necessary or not in that case. The mixer conditions required are generally substantially the same as those required for micronization and granulation, so the mixer need only do what is required.

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 clearly formulation dependent, but is generally in the range 30-45°C, preferably about 35°C.

Similar to the above-mentioned Japanese Patent No. 61069897 A (Kao), it is an essential accomplishment of the present invention that no "surface property improving agent" is contained during granulation. When processing formulations with a relatively high ratio of aluminosilicate molding agent to surfactant, according to the invention, a fine powder material, such as finely divided sodium aluminosilicate, may be used during the granulation step. is not only unnecessary, but can make granulation more difficult or even impossible with any formulation.

Optional Flow Aid According to a preferred embodiment of the invention, a finely ground particulate flow aid may be mixed with the granular material after granulation is complete. The flow aid is conveniently added while the granulate is still in the high speed mixer/granulator and the low speed mixer is run for a further short period of time. No further granulation occurs at this stage. It is also within the scope of the invention to add flow aids to the granular material after it has been transferred to a different device. This embodiment of the invention is disclosed in the above-mentioned Japanese Patent No. 6106, in which a "surface property modifying agent", which may be a finely divided sodium aluminosilicate, is included during the granulation step itself.
It needs to be distinguished from the conventional technical process of No. 9897 A (Kao). It is within the scope of this invention to add particulate flow aids after granulation is complete, but as noted above,
It is essential to the invention that no finely ground particulate material "surface property modifier" is included during granulation. The addition of flow aids after granulation is complete has an additional beneficial effect on the properties of the granulated material regardless of formulation, whereas the presence of such materials during the granulation step in the method of the invention
Processing becomes more difficult.

During subsequent flow aid mixing, the preferred granulation temperature is
It may be maintained at 0-45°C, preferably about 35°C.

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

According to a preferred embodiment of the invention, as described and claimed in our co-pending application of the same date (Case 0°3236), the flow aid is a finely ground amorphous sodium aluminosilicate.

A suitable material is commercially available from Warrlngt On, Cheshlre, UK under the registered trademark Iusil.
It is commercially available from Rosf'eld Chemicals Ltd. This material is effective at very low levels in improving flow properties and also has the ability to increase bulk density. Therefore, the bulk density can be adjusted by appropriately selecting the level of amorphous sodium aluminosilicate added after granulation.

Amorphous sodium aluminosilicate from 0.2 to 5.0% by weight, more preferably from 0.5 to 5.0% by weight, based on the starting powder.
Effectively used in an amount of 3.0% by weight.

Another preferred flow aid is finely divided crystalline sodium aluminosilicate. Crystalline aluminosilicates, previously discussed in connection with molding agents, are also suitable for use as flow aids. However, they have lower weight-potency values than amorphous substances, ranging from 3.0 to 12.0% by weight,
Preferably, it is used in an amount of 4.0 to 10.0% by weight.

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

Other flow aids suitable for use in the process of the invention include precipitated silicic acids, such as Neosil®, and precipitated calcium silicates, such as Microcal®, both of which are Ch
Elcals Ltd, Ltd. (Cheshire, UK)
, Warrington).

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

EXAMPLES Example 1 A detergent composition was prepared by spray drying an aqueous slurry to substantially zero water content and had the following composition: Part linear alkylbenzene 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,
094.64 Note that the ratio of zeolite (anhydrous) to non-crystalline surfactant in this composition was 1.46.

35 kg of this spray-dried powder was introduced into a Fukae® FS-G series high speed mixer/granulator and micronized at high speed for 2-4 minutes. Then water (2,
0 parts) was sprayed while the mixer was running at low speed, then the speed was increased for 5-8 minutes while maintaining the temperature at about 35°C. Granulation occurred during this period.

A sample of the granulated product was removed from the mixer.

It was free-flowing and showed no tendency to cake softening. Its dynamic flow rate was 65 m1/sec.

Arcyl A, a finely shaped amorphous sodium aluminosilicate
The 1 usil 1.0 part was introduced into the Fukae mixer and the mixer was then run on low speed for 1 minute. The resulting granular product was free-flowing and showed no tendency to cake softening. Its bulk density is 74
0 g/liter and its particle porosity was less than 0.20. Its average particle size was 405 microns and its dynamic flow rate was 105 m17 seconds.

The following ingredients were then mixed with the granular material to produce a final detergent powder of 99 parts: Colored pellets 1.5 parts Enzyme (Alcalase) O, at parts Fragrance 0.25 parts Examples 2 and 3 Implementation 20 kg of the spray-dried powder used in Example 1 was
e® FS-30 high speed mixer/granulator and micronized for 4 minutes. Next, water (0.8k
g) was added and the mixture was granulated for 4 minutes while maintaining the temperature at about 35°C. A sample (Example 2) was removed from the mixer and its powder properties were determined; these are shown in Table 1 below.

Finely ground amorphous sodium aluminosilicate Arcil® (0.2 kg) was then added. The physical properties of the resulting powder (Example 3) are shown in Table 1 below, which shows that the addition of flow aids after granulation has no effect on flow and bulk density. The beneficial effects are obvious. When arsyl is contained, <1
The content of 80 micron fine particles increases, but does not increase to unacceptable levels.

Comparative Example A 20 kg of the spray-dried powder used in Example 1 was
e into a high speed mixer/granulator and micronized for 4 minutes. Finely ground amorphous sodium aluminosilicate Arcil® (0.2 kg) was then introduced into the mixer. Water (0.8 kg) was then added and the mixture was granulated for 4 minutes while maintaining the temperature at approximately 35°C. The physical properties of the resulting powder are shown in Table 1 below, from which the disadvantageous effect of adding arsyl before granulation is clear. Note that the increase in particulate content is significantly greater than when arsyl is added before granulation.

Table 1 Example 23A Bulk density 688 740 670 (g/
109 120 80 (ml /
sec) Particle size 550 480 380 (microns) Particulate content 01022 (wt% of powder less than 180 microns) Particle pore dust 0.1 0.1 (Unmeasurable) Comparative example B This comparative example has a high level of shadow. Attempts to implement the method of the invention using different spray drying formulations containing ionic surfactants and relatively low levels of sodium aluminosilicate are described. The formula is as follows; (blank below) Parts Spray Drying Base Linear Alkyl Henzene Sulfonate 2B, 0 Sulfuric 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 sulfate 4.0 Acrylate/malate copolymer 1.0 Moisture
After 4.0 Added zeolite (hydrate) zero 5.0 Sodium carbonate (granules) 15.0 Nonionic surfactant 3.0100.0 Equivalent amount of zeolite (anhydrous) to the anhydrous zeolite in this 3.9 part The ratio of non-toxic surfactant (0,53) is 0.9:
It was less than 1.

Spray-dried base powder (7,7 kg) with Geosna D 1os
15 parts (1,3 kg) of granulated soda ash were placed in a na (R) bowl type high speed mixer/granulator and sprayed with 5,0 parts (0,3 kg) of non-ionic surfactant.
5 kg) and 5 parts of zeolite (0.5 kg) were added. Stirrer speed 196rpm, cutting machine speed 3000r
Micronization was attempted for 1 minute at pm, but the mixture overgranulated resulting in large clumps and overheated.

Examples 4 and 5 35 kg of the spray-dried powder used in Example 1 was added to Regige L.
od! The mixture was introduced into a FM series high speed mixer/granulator and pulverized for 4 minutes.

Then, while the mixer was continuously running at the same speed, water (+,...
1 kg, 35%) and then reduce the temperature to approximately 35°C.
The mixer was run for an additional 3 minutes while maintaining

Granulation occurred during this period. A sample (Example 4) was removed from the mixer and its powder properties were determined; these are shown in Table 2 below.

Finely ground amorphous sodium aluminosilicate Arcil® (1.2 kg) was then introduced into the mixer and it was run for a further 5 minutes. The physical properties of the resulting powder (Example 3) are shown in Table 2 below. The results were similar to those made in Example 2 and Example 3 1) using a Fukae mixer.

Comparative Example C 28.8 kg of the spray-dried powder used in Example 1 was mixed with Resige (
FM series high speed mixer/granulator and pulverized for 4 minutes. Arcil (registered trademark) (1), a finely crushed amorphous sodium aluminosilicate
, 2 kg) were then introduced into the mixer. Water (1.1 kg, 3.5%) was sprayed while the mixer continued to run, then the mixer was run for a further 3 minutes while maintaining the temperature at about 35°C.

Granulation occurred during this period. The physical properties of the resulting powder are shown in Table 2 below.

Table 2 Example 4 5C Bulk density 880 754 704 (
g/liter) Dynamically fluidized dust 100 109 59 (m1
/sec) Particle size 573 524 424 (
Micron) Fine particle content 0 15 25 (< 18
(% by weight of micron particles)) Particle pore size < 0.20 (0,20 (not measurable) Comparative Example: Similar to that used in Comparative Example B, high level of anionic surfactant and relative Using a spray-dried formulation containing low levels of sodium aluminosilicate, Resige Lod
This comparative example describes an attempt to implement the process of the invention in a 1ge mixer. The formulation is as follows: (Left below) Parts linear alkylbenzene sulfonate 26.0 Primary alcohol sulfate 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 water 2.968.9 The ratio of zeolite to non-climate surfactant (0,31) is 0
．． 9: It was less than 1.

The formulation material (30 kg) was placed in a Regige F M mixer and mixed as in Examples 4 and 5 and Comparative Example C.
Run the mixer for a minute. No finely crushed powder in the form of dust was obtained, and it was unclear whether pulverization had occurred. Next, as in the above example, water (1,05 kg, 3.59 kg) was added.
6) was added and granulation was attempted for 0.5 minutes, but the results were questionable.

Examples 6-8 The labeled compositions shown in Example 1 were spray dried to three different moisture contents, as shown in Table 3 below.
Different types of powders were prepared. Since the 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 determined by subtracting that value from the total water content. Note that the powder of Example 6 was overdry, while the powder of Example 8 contained 3.16 parts water.

A 10 kg batch of each powder was granulated (and optionally micronized) in a Geosna® V series mixer at an agitator speed of 298 rpm and a cutter speed of 3000 rpm. In the case of Examples 6 and 7 where micronization occurs first, water was sprayed into the mixer in the amount and time indicated before granulation. After completion of granulation, a finely ground amorphous sodium aluminosilicate, arsil (0.1 kg), was mixed into the granulated material. The properties of the three types of granular materials are shown in Table 3.

Table 3 Examples 78 Total hydraulic power 8.0 11.014.0 (wt-%) Micronization time (min) 4 3 - Water addition amount ckg) 0.2 0.1 - Time (min) 2 1 - Granules Curing time (minutes) 4 3 4 Bulk density
740 832 735 (g/liter) Dynamic flow rate 114 120 12
0 (m1/sec) Compressibility 8.8 9.4 8.8 (96v/ν) Particle size 483 553 521
(microns) Fine particle content 5.0 2.4 8.
1 (wt%<180 microns) Porosity of particles <0.20 (0,20<
0.20 Example 9 This example describes the addition of an additional ingredient (sodium carbonate) to the spray-dried base powder in a mixer prior to micronization and granulation. Its formulation is as follows; Parts Spray Drying Base Linear Alkyl Benzene Sulfonate 24.0 Nonionic Surfactant 2.0 Soap
1.0 zeolite (anhydrous)
3g, 0 zeolite bound water
10.84 Sodium silicate
4.0 acrylate/malate copolymer
2.0 minor ingredients
2.084.04 Sodium carbonate added in mixer 10.094
．． 04 8.5 kg of spray-dried base powder and 1.0 kg of sodium carbonate (light soda ash) were placed in a Geosna v100 mixer and stirrer speed 196 rpI! , cutting machine speed 3000
Micronized for 4 minutes at rpm. Mixer agitator speed 98
rpm.

While operating the cutting machine at a speed of 1500 rpm,
kg) over 2 minutes and then the mixture was stirred at a stirrer speed of 196 rpa+ and a cutter speed of 3000 rpm.
The mixture was granulated for 5 minutes.

Finally, while running the mixer with the stirrer speed 98 rpm and the cutting machine switched off, add Alsil (0,1 kg).
were mixed.

The properties of the resulting bundled granular material are as follows: Bulk density (g/l) 780 Dynamic flow rate (ml/sec) 133 Compressibility (%v/v) ? Particle size (microns) 839 Particle pore size 0.10 The ratio of aluminosilicate to non-crystalline surfactant in the granulated mixture was 1.46.

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

Tuman spray-dried base linear alkylbenzene sulfonate 12.0 Nonionic surfactant 2.0 Soap
1.0 Zeolite (anhydrous) 38.0 Zeolite bound water
10.114 Sodium carbonate (light soda ash) 10.0 Sodium silicate
4.0 acrylate/malate copolymer
2.0 minor component 2.0
81.84 Add linear alkylbenzene sulfonate 12.0 (powder) into a mixer 93.84 Spray-dried base powder 1 f3, 5 kg and linear alkylbenzene sulfonate powder (Markov Marlon (
Registered trademark) A 390 manufactured by Huls) 2.4 kg
into the Geosna V100 mixer and set the stirrer speed to 1.
Micronized for 4 minutes at 911 irpm and cutter speed 3000 rpm. Water (0,45 kg) was added over 2 minutes while the mixer was running at an agitator speed of 98 rpm and a cutter speed of 1500 rpo+, and the mixture was then run at an agitator speed of 196 rpm and a cutter speed of 3000 rpo+.
The mixture was granulated for 5 minutes at rpm. During the granulation period, the temperature was increased to 40°C.
Raised to ℃. Finally, Alcyl (0.19 kg) was mixed in while running the mixer at a stirrer speed of 98 rprn and with the cutter switched off.

The properties of the resulting granular material were as follows: Bulk density (g/liter) 714 Dynamic flow rate (ml/sec) 55 Compressibility (%v/v) 17 Particle size (microns) 712 The ratio of aluminosilicate to non-crystalline surfactant in the mixture subjected to granulation was 1.46.

Examples 11 and 12 These examples involve densifying and granulating powders prepared by dry mixing in a high speed mixer/granulator. Prepare the following formulations by mixing in a concrete mixer: Part Linear Alkyl Benzene Sulfonate 24.0 Nonionic Surfactant 2.0 Soap
1.0 zeolite (anhydrous) 3B,0 zeolite bound water
10.84 Sodium carbonate (light soda ash) 10.0 Sodium silicate
4.0 Acrylate/malate copolymer 2.0 Minor acid content
2,092.24 The ratio of aluminosilicate to non-climate surfactant in this mixture was 1.46.

20 kg of the formulated substance was placed in a Geosna V10O mixer, stirrer speed 196 rp11 and cutter speed 3000.
Mixed for 1 minute at rpm. The mixer has an agitator speed of 9
Water (0.2 kg) was added over 2 minutes while operating at 8 rpm and cutter speed 1500 rpm and the mixture was then granulated for 4 minutes at stirrer speed 196 rpm and cutter speed 3000 rpm. Specimen (Example 11
), and its powder properties were determined as #lP1 (see below).

Finally, while running the mixer at a stirrer speed of 98 rpIll and with the cutter switched off, add Alsil (0,2
kg) and the powder properties of the final granulated material (Example 12) were also determined.

The powder properties of the granular material before and after the addition of arsyl were as follows: Bulk density Cg/liter) 780 810 Dynamic flowability (ml/s) 80 9B Compressibility (
%v/v) 17.0 15.3 Particle size (microns) -607 Porosity
<0.20 <0.20 Example 13 The following formulations were prepared by dry mixing method using a Fukae FS-1200 mixer:
(Left below) The ingredients listed in the "Brimix" section were mixed in a Fukae mixer at a stirrer speed of 80 rpm and a cutter speed of 200 rpm.
Mix for 2 minutes at m. The nonionic surfactant was then added over a period of 1 minute, followed by water over a 2 minute period with the mixer running at the same agitator and cutter speeds. This was followed by granulation for 6 minutes at the same speed and finally the zeolite was added for 2 minutes still at the same speed.

The properties of the resulting granular material were as follows: Bulk density (g/liter) 780 Dynamic flow rate (ml/sec) 83 Compressibility (%v/v) 11.8 Particle size (microns) ) 477 Particle Pore Chenpi 0.1 The ratio of zeolite (anhydrous) to non-lethal detergent active in the granulated material was 1.0.

Claims (5)

[Claims] (1) A granular detergent composition, or component thereof, having a bulk density of at least 650 g/liter, preferably at least 700 g/liter, and a powder porosity of less than 0.25, preferably less than 0.20, comprising: (a) 17-35% by weight of a non-soap cleaning active, at least in part consisting of an anionic cleaning active; and (b) 28-45% by weight (anhydrous basis) of crystalline or amorphous aluminosilicate. containing sodium, the weight ratio of (b):(a) being from 0.9:1 to 2.6:1, preferably from 1.2:1 to 1.8:1, and any other detergents. The said composition is made up to 100% by weight with the ingredients added. (2) a method for producing a granular detergent composition or ingredient having a bulk density of at least 650 g/liter, preferably at least 700 g/liter, and a powder porosity of less than 0.25, preferably less than 0.20; (a) 5 to 35% by weight, preferably 17 to 35% by weight of non-soapy cleaning actives consisting at least in part of anionic cleaning actives, and (b) 28 to 45% by weight of anhydrous (b):(a) weight ratio of at least 0.9:1, preferably 0.9:1 to 2.6:1, and 100% The granular starting material with any other detergent ingredients added in weight percent is added in a high speed mixer/granulator with stirring and cutting functions in the presence of a liquid binder.
A process comprising processing in the absence of a finely divided particulate surface property modifier, thereby granulating and densifying to a bulk density of at least 650 g/l. (3) A method according to claim 2, in which the granulation is carried out in a bowl-shaped high speed mixer/granulator having a substantially vertical stirring shaft. 4. The method of claim 2, wherein the particulate starting material at least partially comprises a spray-dried powder. 5. The method of claim 2, wherein the granular starting materials are prepared, at least in part, by mixing in a high speed mixer/granulator followed by granulation.