WO2012157681A1

WO2012157681A1 - Process for manufacturing group of detergent granules

Info

Publication number: WO2012157681A1
Application number: PCT/JP2012/062536
Authority: WO
Inventors: 中山　高志; 浩章割田; 今泉　義信; 将寛山口
Original assignee: 花王株式会社
Priority date: 2011-05-18
Filing date: 2012-05-16
Publication date: 2012-11-22
Also published as: JP2012255145A; CN103547665A; CN103547665B

Abstract

A process for manufacturing a group of detergent granules which includes a step of granulating powdery raw materials for a detergent in a rotating mixer, wherein the granulation of the powdery raw materials is conducted with a foamed anionic surfactant composition sprayed in the rotating mixer through a multi-fluid nozzle. By this process, a group of detergent granules having a medium or low bulk density can be obtained in a high yield. The group of detergent granules thus obtained exhibits high solubility.

Description

Method for producing detergent particles

The present invention relates to a method for producing a detergent particle group using a container rotating mixer, a foam of an anionic surfactant composition, and a multi-fluid nozzle.

Currently available detergents are roughly classified into high bulk density detergents (greater than 690 g / L), medium bulk density detergents (400 to 690 g / L), and low bulk density detergents (250 g / L to 400 g). / L) and liquid detergents. For example, high bulk density detergents are often used in Japan, but there are also many demands for medium and low bulk density detergents in Asia, Oceania and Europe.

From the viewpoint of economy and environmental friendliness, a method for producing a detergent composition using an anionic surfactant by a non-spray drying method is disclosed as a production method not using spray drying. Patent Document 1 discloses a method of continuously producing a detergent composition using a surfactant paste and a dried detergent material in a high speed mixer / medium speed mixer / dryer. Patent Document 2 discloses a method for continuously producing a detergent composition while recirculating fine particles of a surfactant paste and a dried detergent raw material with a high speed mixer / medium speed mixer / conditioning device.

However, it is difficult to adjust the particle size in the manufacturing method of Patent Document 1, and the manufacturing method of Patent Document 2 uses a manufacturing method in which fine particles are recirculated in order to adjust the particle size, which is a manufacturing method with low productivity. . Therefore, there is a demand for a production method that can easily obtain a detergent particle group having a required particle size with a high yield. Furthermore, all of these patent documents provide a method for increasing the bulk density of detergent particles, and are not suitable as a method for producing a group of medium and low bulk density detergent particles.

Patent Document 3 discloses a method for producing surfactant granules by introducing a foam of a surfactant into a mixer as a production method for reducing or not using spray drying.

However, the production method of Patent Document 3 is insufficient as a production method for obtaining detergent particles in good yield.

Japanese National Patent Publication No. 10-500716 Japanese National Patent Publication No. 10-506141 Special table 2002-525420 gazette

The present invention is a method for producing detergent particles having a step of granulating a powder raw material for detergent using a container rotating mixer,
The present invention relates to a method for producing a detergent particle group in which a foam of an anionic surfactant composition is sprayed into the container rotary mixer using a multi-fluid nozzle to granulate the detergent powder raw material. .

Detailed Description of the Invention

The present invention relates to providing a method for producing a medium / low bulk density detergent particle group containing an anionic surfactant with high yield without using spray drying.

According to the method for producing detergent particles of the present invention, there is an effect that a detergent particle group having a medium to low bulk density can be obtained with good yield. The medium and low bulk density detergent particles obtained in this way also have the effect of exhibiting high solubility.

One of the features of the present invention is that the powder raw material for detergent is granulated using a rotating container mixer.

In general, in granulation using a rotating container mixer, it is possible to make the powder flow uniformly, and because of the mixing mechanism involving lifting of the particles by rotation and sliding / falling by their own weight, The shearing force applied to is suppressed. Therefore, it can be said that the granulation method using such a mixer is a non-consolidated granulation method. In addition, since the anionic surfactant composition added to such a mixer does not progress in granulation unless the adhesiveness when it comes into contact with the powder is strong, the adhesiveness develops when it comes into contact with the powder. There is a need. When such an anionic surfactant composition is supplied to a container rotation type mixer by a one-fluid nozzle or pipe, which is a general supply method, it is difficult to uniformly disperse the supplied liquid component in the mixer. There is a tendency that coarse particles are likely to be formed due to the large liquid mass generated in nature.

Thus, when a multi-fluid nozzle such as a two-fluid nozzle is used and sprayed with a foam of an anionic surfactant composition that develops an adhesive property when it comes into contact with the powder, it is supplied into the container rotary mixer. Surprisingly, it was found that uniform granulation can be achieved while suppressing the formation of coarse particles. This is because the foam of such an anionic surfactant composition is made into fine droplets in advance using a multi-fluid nozzle so that the anionic surfactant composition can be obtained even in a container-rotating mixer. It is considered that high dispersion of the foam can be achieved and a large liquid mass forming coarse particles is not generated. Therefore, detergent particles can be produced in a high yield by adding a foam of an anionic surfactant composition that exhibits adhesiveness when it comes into contact with the powder into a rotating container mixer using a multi-fluid nozzle. can do.

Furthermore, one of the features of the present invention is that the foam of the anionic surfactant composition is sprayed using a multi-fluid nozzle.

When the anionic surfactant composition is made into a foam, it not only exhibits adhesiveness when in contact with the powder, but also reduces the specific gravity. When such a foam is sprayed using a multi-fluid nozzle, fine droplets having a reduced specific gravity are generated and the number thereof is increased. As a result, the volume of the anionic surfactant composition per detergent particle increases in the granulation with the detergent powder raw material, and the anionic surfactant composition is a foam. Since the specific gravity is reduced, the density per detergent particle is reduced as compared with the case where the anionic surfactant composition is not made into a foam, so that a detergent particle group having a medium to low bulk density can be obtained. it can.

As described above, in the present invention, a combination of a container rotating type mixer and a multi-fluid nozzle is adopted, and further, a foam of an anionic surfactant composition is used. An effect of obtaining a detergent particle group having a medium to low bulk density with high yield is obtained.

As an aspect of the granulation in the production method of the present invention, the foam of the anionic surfactant composition is stirred using the multi-fluid nozzle while stirring the powder raw material for the detergent using a container rotating mixer. If it is the aspect sprayed on this powder raw material for detergents, it will not specifically limit. Hereinafter, the aspect as an example of the manufacturing method of this invention is demonstrated in detail.

In the present invention, the detergent particles are particles containing a surfactant and a builder, and the detergent particle group means an aggregate thereof. The detergent composition contains detergent particles and is optionally added separately from the detergent particles (for example, builder granules, fluorescent dyes, enzymes, fragrances, antifoams, bleaches, bleach activators) Etc.).

In this specification, water-soluble means that the solubility in water at 25 ° C. is 0.5 g / 100 g or more, and water-insoluble means that the solubility in water at 25 ° C. is less than 0.5 g / 100 g. Means.

A. Detergent Particle Group The detergent particle group of the present invention comprises (1) a powder raw material for detergent and (2) a foamed anionic surfactant composition. The detergent particle group of the present invention may further contain (3) other powder components and / or (4) other liquid components.

(1) Powder raw material for detergent The powder raw material for detergent includes a water-soluble solid alkali inorganic substance and / or a water-soluble inorganic salt.

(1-1) Water-soluble solid alkali-inorganic substance The water-soluble solid alkali-inorganic substance is an alkali inorganic substance that is solid at room temperature (20 ° C.), and the water-soluble solid alkali-inorganic substance is not particularly defined. Examples thereof include sodium carbonate, sodium hydrogen carbonate, potassium carbonate, sodium silicate and the like. Among them, sodium carbonate is preferable as an alkaline agent that exhibits a suitable pH buffer region in the washing liquid. These water-soluble solid alkali inorganic materials may be used alone or in combination of two or more.

As sodium carbonate, either light soda ash (light ash) or heavy soda ash (dense ash) can be used.

Further, the average particle diameter of the water-soluble solid alkali inorganic substance is not particularly limited, but when the surfactant is highly blended, it may be pulverized to 1 to 50 μm from the viewpoint of improving the yield. The average particle size of the water-soluble solid alkali inorganic substance is calculated on a volume basis, and is measured using, for example, a laser diffraction particle size distribution analyzer: LA-920 (manufactured by Horiba, Ltd.). Value.

(1-2) Water-soluble inorganic salt The water-soluble inorganic salt is preferably used as a powder raw material for detergents in order to increase the ionic strength of the washing liquid and improve the effects of cleaning sebum dirt. As the water-soluble inorganic salt, for example, sodium sulfate, sodium chloride, sodium sulfite and potassium sulfate having a high degree of ionic dissociation are preferable. From the viewpoint of improving the dissolution rate, the combined use of magnesium sulfate is also effective.

Further, the average particle size of the water-soluble inorganic salt is not particularly limited, but when an anionic surfactant is highly blended, it may be pulverized to 1 to 50 μm from the viewpoint of improving the yield of the detergent particles. . The average particle diameter of the water-soluble inorganic salt is calculated on a volume basis. For example, it is a value measured using a laser diffraction particle size distribution analyzer: LA-920 (manufactured by Horiba, Ltd.). is there.

As the powder raw material for detergent, among the water-soluble solid alkali inorganic substance and the water-soluble inorganic salt, the exemplified raw materials may be used alone, or two or more kinds may be mixed and used. The powder raw material for detergent is preferably sodium carbonate and / or sodium sulfate, and more preferably light ash.

In the detergent particle group, the content of the powder raw material for the detergent, preferably the content of the water-soluble solid alkali inorganic substance and the water-soluble inorganic salt is preferably 10% by mass or more, and 20% by mass or more from the viewpoint of improving detergency. Is more preferable. Moreover, 80 mass% or less is preferable from a viewpoint of the reduction of the bulk density of a detergent particle group. From these viewpoints, the content of the powder raw material for the detergent in the detergent particle group, preferably the content of the water-soluble solid alkali inorganic substance and the water-soluble inorganic salt is preferably 10 to 80% by mass, and 20 to 80% by mass. % Is more preferable.

(2) Foam of anionic surfactant composition (2-1) Anionic surfactant composition As the anionic surfactant composition used in the present invention, a viewpoint of obtaining detergent particles having a sharp particle size distribution Therefore, a surfactant paste is preferable, and a surfactant paste containing the following components a) and b) is more preferable.

a) One or more anionic surfactants selected from the group consisting of salts of linear alkylbenzene sulfonic acids, salts of alkyl sulfates and salts of polyoxyethylene alkyl sulfates.
b) 25 to 70 parts by weight of water with respect to 100 parts by weight of component a) above.

As the salt of the linear alkylbenzene sulfonic acid, the alkyl group preferably has 10 to 18 carbon atoms, more preferably 12 to 16 carbon atoms. Examples of the salt include Na salt, K salt, ammonium salt, and amine salt. As the salt of the alkyl sulfate, an alkyl group or an alkenyl group having 10 to 18 carbon atoms, more preferably 12 to 16 carbon atoms in the carbon chain is preferable. Examples of the salt include Na salt, K salt, ammonium salt, and amine salt.

The polyoxyethylene alkylsulfuric acid salt is preferably an alkyl or alkenyl group having 10 to 18 carbon atoms, more preferably 12 to 16 carbon atoms in the carbon chain. Further, the average added mole number of polyoxyethylene is preferably 0.1 to 3.0. Further, examples of the salt include Na salt, K salt, ammonium salt or amine salt.
Among these, from the viewpoint of obtaining detergent particles having a sharp particle size distribution, alkyl sulfate salts are preferred.

The surfactant paste contains at least an anionic surfactant shown as the component a) and water shown as the component b). The paste at 60 ° C. preferably has a viscosity of 100 Pa · s or less.

The viscosity of the surfactant paste varies greatly depending on its water content. For example, the surfactant paste can be prepared by neutralizing the acid precursor of component a) with an alkali compound. At this time, the water content of the alkali compound used is adjusted to have a desired moisture content. That is, it is preferable to prepare a surfactant paste having a desired viscosity. When the anionic surfactant contains 25 to 70 parts by mass of water with respect to 100 parts by mass of the anionic surfactant, it becomes a paste-like anionic surfactant having a reduced viscosity and is easy to handle. In the present invention, it is preferable to use a surfactant paste in which the water content of the anionic surfactant is adjusted.

The range of the amount of water in the surfactant paste is preferably 25 to 70 parts by weight, more preferably 30 to 65 parts by weight, and more preferably 35 to 65 parts by weight with respect to 100 parts by weight of component a) from the viewpoint of handling. More preferably, the water content in the surfactant paste is preferably 20 to 41% by mass, more preferably 23 to 39% by mass, and even more preferably 26 to 39% by mass from the viewpoint of handling.

In addition, the viscosity of the surfactant paste is preferably 10 Pa · s or less, more preferably 5 Pa · s or less, preferably from the viewpoint of handleability in production, preferably in the use temperature range of the surfactant paste. Preferably, it is 0.5 Pa · s or more, more preferably 1 Pa · s or more. From these viewpoints, it is preferably 0.5 to 10 Pa · s, and more preferably 1 to 5 Pa · s. The use temperature range is preferably 20 to 70 ° C., more preferably 20 to 60 ° C., from the viewpoint of the stability of the surfactant paste. Here, the viscosity is determined by measuring at a shear rate of 50 [1 / s] with a coaxial double cylindrical rotational viscometer (manufactured by HAAKE, sensor: SV-DIN).

The method for preparing the surfactant paste is not particularly limited, and a known method can be used. Among the acid precursors of the anionic surfactant, those which are very unstable and easily decomposed are preferably prepared so that the decomposition can be suppressed. For example, using a loop reactor, the heat of neutralization is removed by a heat exchanger or the like, and the production may be performed while paying attention to the temperature control of the acid precursor and the surfactant paste. The temperature range during production is preferably 30 to 60 ° C., and the storage temperature range after production is preferably 60 ° C. or less. Further, at the time of use, the temperature may be raised as necessary, and a surfactant paste may be used.

The obtained surfactant paste preferably has an excessive alkalinity from the viewpoint of suppressing decomposition.

The surfactant paste includes unreacted alcohol and unreacted polyoxyethylene alkyl ether at the time of producing the acid precursor, sodium sulfate as a by-product during the neutralization reaction, and a pH buffer that can be added during the neutralization reaction Further, a decolorizing agent or the like may be contained.

In the surfactant paste, one or more of the component a) can be used alone as the surfactant, but the following surfactants can also be used in combination. When using together, you may mix and use the surfactant paste containing a) component previously, and you may add separately, respectively. When the following surfactant is used in combination, the following surfactant is preferably 1 to 70 parts by weight, more preferably 2 to 50 parts by weight, and still more preferably 3 to 30 parts per 100 parts by weight of component a). Part by mass. Examples of such surfactants include α-sulfo fatty acid ester salts and secondary alkane sulfonates.

(2-2) Foam In the present invention, a foam of the above anionic surfactant composition is used. The foam is obtained by containing a gas medium (air, nitrogen, carbon dioxide, etc.) in the anionic surfactant composition. As the gas medium, air (air) is preferable from the viewpoint of productivity.

Such a foam can be obtained, for example, by mixing a gas medium into an anionic surfactant composition. More specific methods for preparing the foam include a batch method and a continuous method. As a batch type, the anionic surfactant composition is put into a kneader generally used such as a batch kneader, and the gas medium is entrained by performing kneading for a predetermined time in the presence of the gas medium. It is a method of preparing.

The continuous method is a method of preparing a foam by mixing and dispersing a gas medium by continuously introducing a predetermined amount of the surfactant composition and the gas medium into a high-speed rotating part.

The continuous preparation method is preferred from the viewpoints of stability of physical properties such as specific gravity of the foam, ease of preparation method, and productivity. As an example of the foaming machine which performs such a continuous preparation method, there are MDF series (manufactured by Taihei Kiko Co., Ltd.), BM series (manufactured by Yana Gear Co., Ltd.) and the like.

In the batch-type preparation method, the specific gravity of the foam can be controlled by the kneading time of the surfactant composition.

In the continuous preparation method, the specific gravity of the foam can be controlled by adjusting the flow rate of the gas medium with respect to the surfactant composition. The range of the volume flow rate of the gas medium is preferably, for example, in the range of 0.2 to 10 times the volume flow rate of the surfactant composition. The gas medium is preferably mixed into the anionic surfactant using a foaming machine.

The temperature of the anionic surfactant composition at the time of supplying to the foaming machine is preferably 20 to 70 ° C., more preferably 20 to 60 ° C., from the viewpoint of the stability of the surfactant paste.

The specific gravity of the resulting foam of the anionic surfactant composition is preferably 0.1 to 0.9, more preferably 0.1 to 0.9, from the viewpoint of obtaining a medium / low bulk density detergent particle group in good yield. 0.8, more preferably 0.1 to 0.7.

In addition, as content of the anionic surfactant in the detergent particle group obtained by this invention, it is 5 mass% in detergent particle group from a viewpoint of forming a granulated material with a cleaning power and the powder raw material for detergents. The above is preferable, and 10 mass% or more is more preferable. Further, from the viewpoint of suppressing the generation of coarse particles, it is preferably 50% by mass or less, more preferably 40% by mass or less. From these viewpoints, the content in the detergent particle group is preferably 5 to 50% by mass, 10 to 50% by mass is more preferable, and 10 to 40% by mass is even more preferable.

In the present invention, (2) the foam of the anionic surfactant composition has the ability to form a granulated product by combining powder raw materials for detergent, and as described in the above paragraph, One feature of the present application is that the anionic surfactant composition exhibits adhesiveness when it comes into contact with the powder raw material for detergent.

When the foam of the anionic surfactant composition is added to the detergent powder raw material, the moisture in the anionic surfactant composition is deprived by the hydration or dissolution of the detergent powder raw material. Or when the temperature of the detergent powder raw material is lower than the temperature of the anionic surfactant, the temperature of the foam of the anionic surfactant composition decreases to near or below its melting point. Thus, it is presumed that the anionic surfactant composition foam is solidified to develop adhesiveness.

As described above, when the foam of the anionic surfactant composition comes into contact with the detergent powder raw material, it develops an adhesive property, whereby granulation of the detergent powder raw material proceeds. As a standard of expression, the viscosity of the foam of the anionic surfactant composition when it comes into contact with the powder raw material for detergent is preferably 2 Pa · s or more, more preferably 3 Pa · s or more. The viscosity of the foam at the time of contact was determined by the anionic surfactant under the condition of a shear rate of 50 [1 / s] using a coaxial double cylindrical rotational viscometer (manufactured by HAAKE, sensor: SV-DIN). What is necessary is just to adjust and measure the temperature and moisture value so that it may become the same as when the foam of a composition contacts the powder raw material for detergents.

(3) Other powder components In addition to the "powder raw material for detergents", generally known substances generally used in the field of detergent compositions may be added to the container rotary mixer. The amount of the other powder component in the detergent particle group is preferably 1 to 30% by mass, and more preferably 1 to 20% by mass.

Such substances include chelating agents (tripolyphosphates, orthophosphates, pyrophosphates, alkali metal aluminosilicates), powders of water-soluble polymers (carboxylic acid polymers, carboxymethylcellulose, soluble starch, saccharides, Polyethylene glycol), water-insoluble excipients (silicon dioxide, hydrated silicate compounds, clay compounds such as barlite, bentonite, etc.), particulate surfactants (fatty acids or salts thereof, linear alkylbenzene sulfonates, alkyls) Sulfate, etc.).

The above substances may be added together with the powder raw material for the detergent before adding the foam of the anionic surfactant composition, or the foam of the anionic surfactant composition may be added. It may be added after. When adding an alkali metal aluminosilicate, it can be used as a surface modifier to improve fluidity and storage stability, so after adding the foam of the anionic surfactant It is preferable to add.

(4) Other liquid components In the present invention, other liquid components may be added to produce detergent particles. Other liquid components to be added can be appropriately selected according to the composition of the detergent particle group to be obtained. The addition timing of the liquid component is not particularly limited. For example, the liquid component may be mixed in advance with the anionic surfactant composition, or before the foam of the anionic surfactant composition is added. Alternatively, it may be performed during or after that, but when a surface modifier is added, it is preferably before the addition of the surface modifier.

When the liquid component is added after adding the foam of the anionic surfactant composition, the liquid component may be added using a container rotating mixer, or the detergent obtained by the production method of the present invention. After discharging the particle group from the container rotating mixer, the detergent particle group obtained in another mixer / granulator may be charged and the liquid component added thereto.

Examples of the liquid component include any liquid component used in ordinary detergent compositions such as nonionic surfactants, fatty acids, and water-soluble polymers (such as carboxylic acid polymer, carboxymethyl cellulose, soluble starch, saccharide, and polyethylene glycol). It is done. As the liquid component, only one component may be used, or two or more components may be used in combination. The liquid component may be added as a liquid at a temperature equal to or higher than its melting point, or may be added in the form of an aqueous solution or dispersion. The amount of the net liquid component excluding the medium is preferably 15% by mass or less, and more preferably 10% by mass or less of the detergent particle group as the final product, from the viewpoint of suppressing aggregation of the detergent particle group.

The nonionic surfactant used as the liquid component is not particularly limited, but from the viewpoint of detergency, for example, a polyoxyalkylene alkyl obtained by adding 6 to 22 moles of alkylene oxide to an alcohol having 10 to 14 carbon atoms. Ether is preferred.

As a method for adding these liquid components, spraying can be performed with any nozzle, not depending on the multi-fluid nozzle described in the present invention.

B. Method for Producing Detergent Particle Group In the production method of the present invention, a powder raw material for detergent is granulated by spraying a foam of an anionic surfactant composition into the mixer using a container rotating mixer. The process of carrying out. When the foam of the anionic surfactant composition is added, granulation is performed by spraying into the container rotary mixer using a multi-fluid nozzle.

The amount of foam of the anionic surfactant composition to be sprayed is preferably 20 to 100 parts by mass, more preferably 25 to 90 parts by mass with respect to 100 parts by mass of the powder raw material for detergent. 20 parts by mass or more is preferable from the viewpoint of detergency, and 100 parts by mass or less is preferable from the viewpoint of granulation yield and solubility.

(1) Container rotation type mixer As the container rotation type mixer, a drum type mixer or a pan type mixer is preferable. The drum-type mixer is not particularly limited as long as the drum-shaped cylinder rotates and performs processing. In addition to the drum-type mixer that is horizontally or slightly inclined, the conical drum-type granulator is used. (Mixer), multi-stage conical drum granulator (mixer), etc. can also be used. These apparatuses can be used in both batch and continuous processes.

If the coefficient of wall friction between the detergent particle group and the inner wall of the container rotating mixer is small and it is difficult to apply sufficient lifting force to the detergent particle group, a plurality of baffle plates (baffles ( ) May be attached. This makes it possible to cause the particle group to perform an upward movement, and improves the powder mixing property and the solid-liquid mixing property.

The operating condition of the container rotation type mixer is not particularly limited as long as the components in the mixer can be stirred. However, the operating condition is that the fluid number defined by the following formula is 0.005 to 1.0. An operating condition of 0.01 to 0.6 is more preferable.

Fluid number: Fr = V ² / (R × g)
V: Circumferential speed [m / s]
R: Radius from the center of rotation to the circumference of the rotating object [m]
g: Gravity acceleration [m / s ² ]

(2) Multi-fluid nozzle In the present invention, one feature is that the foam of the anionic surfactant composition is supplied using a multi-fluid nozzle. By using such a nozzle, even a fluid component having a relatively high viscosity, such as the above-described surfactant paste or foam thereof, can be used to make the droplets finer and disperse. A multi-fluid nozzle is a nozzle that mixes and atomizes a liquid and atomizing gas (air, nitrogen, etc.) through an independent channel to the vicinity of the nozzle tip. A four-fluid nozzle or the like can be used. Among these multi-fluid nozzles, a two-fluid nozzle is preferable from the viewpoint of ease of operation and availability.

In the present invention, the foam of the anionic surfactant composition and the atomizing gas are preferably mixed and atomized. The type of the mixing part of the foam of the anionic surfactant composition and the gas for atomization is either an internal mixing type that mixes inside the nozzle tip or an external mixing type that mixes outside the nozzle tip. Also good.

As such a multi-fluid nozzle, an internal mixed type two-fluid nozzle such as manufactured by Spraying Systems Japan Co., Ltd., manufactured by Kyoritsu Alloy Manufacturing Co., Ltd., or manufactured by Ikeuchi Co., Ltd., manufactured by Spraying Systems Japan Co., Ltd. And an external mixing type two-fluid nozzle manufactured by Kyoritsu Alloy Mfg. Co., Ltd. and Atmax Co., Ltd., an external mixing type four-fluid nozzle manufactured by Fujisaki Electric Co., Ltd., and the like.

Moreover, the droplet diameter of the foam droplet of the anionic surfactant composition can be adjusted by changing the balance between the flow rate and the flow rate of the atomizing gas. That is, as the flow rate of the atomizing gas is increased with respect to the foam of the anionic surfactant composition having a certain flow rate, the droplet diameter becomes smaller. Furthermore, the droplet diameter becomes smaller as the flow rate of the foam of the anionic surfactant composition is decreased with respect to the atomizing gas at a certain flow rate. As the droplet diameter is smaller, that is, as the flow rate of the atomization gas is increased, the refined droplets can reduce coarse particles, that is, improve the yield.

On the other hand, the foam is subjected to a shearing force by the atomizing gas supplied to the multi-fluid nozzle, and the foam is likely to break up and the specific gravity of the foam is likely to increase. Therefore, it is preferable to adjust the flow rate of the atomizing gas supplied to the multi-fluid nozzle so that an increase in the specific gravity of the foam can be suppressed. That is, in the present invention, there is a suitable atomization gas flow rate in order to achieve both reduction of coarse particles and suppression of increase in the specific gravity of the foam.

The flow rate of a suitable atomizing gas varies depending on the type of multi-fluid nozzle to be used, but [volume flow rate of foam of an anionic surfactant composition (cm ³ / min)] / [flow rate of atomizing gas ( L / min)], it is preferably 0.5 to 30 cm ³ / L, more preferably 1 to 20 cm ³ / L from the viewpoint of obtaining a medium / low bulk density detergent particle group with good yield. is there. The above range is suitable when using a two-fluid nozzle BN90 manufactured by Atmax Co., Ltd.

The droplet diameter of the foam of the anionic surfactant composition after spraying with a multi-fluid nozzle is preferably 10 to 500 μm in average particle diameter.

In addition, the average particle diameter of the droplet diameter of the foam of the anionic surfactant composition is calculated on a volume basis, and a laser diffraction particle size distribution analyzer: Spray Tech (manufactured by Malvern) is used. The value to be measured.

The specific gravity of the foam of the anionic surfactant composition after spraying with a multi-fluid nozzle is preferably from 0.1 to 0.95, more preferably from the viewpoint of obtaining a detergent particle group with medium to low bulk density in good yield. Is from 0.2 to 0.95, more preferably from 0.2 to 0.85.

In addition, when it is desired to increase the rate of addition of the foam of the anionic surfactant composition, it is also effective to use a plurality of these multi-fluid nozzles and increase the rate of addition while maintaining finer droplets. Is.

By using a method in which such a container rotating mixer, an anionic surfactant foam, and a multi-fluid nozzle are combined, even an anionic surfactant foam can be uniformly dispersed. Thus, a medium and low bulk density detergent particle group with improved yield is obtained.

C. Detergent Composition Containing Detergent Particle Group and Method for Producing the Same The detergent particle group produced as described above can be handled as a detergent composition as it is, but a composition to which a desired component is added is also used as a detergent composition. Can be handled. That is, the detergent composition of the present invention contains at least the detergent particles obtained by the production method of the present invention.

Examples of components to be added include builder granules, fluorescent dyes, enzymes, fragrances, antifoaming agents, bleaching agents, bleach activators and the like. Such components may be added to the container rotating mixer after the addition of the anionic surfactant composition, or the detergent particles obtained by the production method of the present invention are removed from the container rotating mixer. After discharging, another mixer may be used for addition.

D. Physical properties and evaluation The physical properties of the detergent particles obtained by the present invention include bulk density, fluidity, and average particle size. Moreover, a granulation yield is mentioned as a physical property used as an index of productivity. In addition, examples of physical properties that serve as an index of solubility include a dissolution rate for 60 seconds and a roughness disappearance time. The bulk density of the detergent particles is preferably a medium to low bulk density of 250 to 690 g / L, more preferably 250 to 650 g / L, and more preferably 300 to 600 g / L, from the viewpoint of excellent dissolution rate for 60 seconds and roughness disappearance time. L is more preferable. The average particle size of the detergent particles is preferably 200 to 800 μm, more preferably 200 to 600 μm from the viewpoint of improving the granulation yield of the detergent particles. The fluidity of the detergent particles is preferably 4 to 12 seconds, more preferably 4 to 10 seconds, and still more preferably 4 to 8 seconds, from the viewpoint of excellent handling of the detergent particles. The granulation yield is preferably as close to 100% as possible, for example, 80 to 100% is preferable, and 90 to 100% is more preferable.

A method for measuring physical properties of the detergent particle group and the like is as described below.
<Method of measuring physical properties>
1. Bulk density The bulk density is measured by the method described as an apparent density in JIS K 3362: 2008. The bulk density is measured with the remaining particles obtained by cutting the particles remaining on the 2000 μm sieve.

2. Fluidity Fluidity is defined as the time required for 100 mL of powder to flow out from the apparent density measurement hopper described in JIS K 3362: 2008. If the powder does not flow out within 60 seconds due to bridging or the like in the hopper, the fluidity is 60 <. In addition, fluidity | liquidity is measured with the remaining particle | grains which cut | disconnected the particle | grains which remained on the 2000 micrometer sieve.

3. Average particle diameter As for the average particle diameter, it was vibrated for 5 minutes using a metal mesh sieve (mesh opening 2000 to 45 μm) described in JIS Z 8801-1: 2006, and then the median diameter was determined from the mass fraction according to the size of the mesh. Is calculated. More specifically, using a 12-stage sieve having a mesh opening of 45 μm, 63 μm, 90 μm, 125 μm, 180 μm, 250 μm, 355 μm, 500 μm, 710 μm, 1000 μm, 1410 μm, and 2000 μm, a small sieve with a mesh on the tray Stack in order, add 100 g of particles from the top of the top 2000 μm sieve, cover and attach to a low-tap sieve shaker (manufactured by HEIKO, tapping 156 times / minute, rolling: 290 times / minute) After vibrating for 5 minutes, the mass of the particles remaining on each sieve and the saucer is measured, and the mass ratio (%) of the particles on each sieve is calculated. The average particle size is obtained by accumulating the mass ratios of the particles on the sieve having a small mesh size in order from the saucer to give a total of 50%.

Further, the value of the percentage of detergent particles remaining on each sieve having an opening of 1000 μm, 1410 μm, and 2000 μm when the average particle size of the detergent particles is measured is obtained as a coarse particle (1000 μm ON) rate. Similarly, the value which represented the ratio of the detergent particle group which remain | survives on a saucer and each sieve with an opening of 45 micrometers, 63 micrometers, and 90 micrometers in mass% is calculated | required as a fine powder (125 micrometers PASS) rate.

4). Granulation yield The granulation yield in this invention shows the ratio in the mass of the particle | grains below 2000 micrometers in the manufactured detergent particle group.

5. Dissolution rate for 60 seconds The dissolution rate for 60 seconds is calculated by the following method.
1 liter of hard water (Ca / Mg molar ratio 7/3) adjusted to 10 ° C. corresponding to a hardness of 71.2 mg CaCO ₃ / liter, 1 liter beaker (inner diameter 105 mm, height 150 mm cylindrical type, for example, manufactured by Iwaki Glass Co., Ltd.) Filled in a 1 liter glass beaker, and kept at a water temperature of 10 ° C. in a water bath, a stirrer (length 35 mm, diameter 8 mm, for example, model: ADVANTEC, Teflon (registered trademark) SA ( In the round thin type)), stirring is performed at a rotational speed (800 r / m) at which the depth of the vortex with respect to the water depth is approximately 1/3. The detergent particles, which have been reduced and weighed so as to be 1.000 ± 0.0010 g, are charged and dispersed in water with stirring, and stirring is continued. 60 seconds after the addition, the detergent particle group dispersion in the beaker was filtered through a metal mesh screen (diameter: 100 mm) having a mesh size of 74 μm described in JIS Z8801-1: 2006, and the water content remaining on the sieve. The detergent particles are collected together with a sieve in an open container of known mass. The operation time from the start of filtration until the sieve is collected is 10 ± 2 seconds. The collected residue of detergent particles is dried in an electric dryer heated to 105 ° C. for 1 hour, and then cooled in a desiccator (25 ° C.) containing silica gel for 30 minutes. After cooling, the total mass of the dry detergent residue, sieve and collection container is measured, and the dissolution rate (%) of the detergent particle group is calculated by the equation (1).

Dissolution rate (%) for 60 seconds = {1− (T / S)} × 100 (1)
S: input mass of detergent particles (g)
T: Dry mass (g) of dissolved residue of detergent particles remaining on the sieve when the aqueous solution obtained under the above stirring conditions is applied to the sieve.

6). Roughness disappearance time The roughness disappearance time is measured by the following method.
When 3 L of water at 20 ° C. is put into a washbasin having a diameter of 35 cm and a depth of 12 cm, and after gently adding 15 g of detergent particles into the washbasin, the bottom of the washbasin is rubbed at a rate of once per second with a palm. The time (in seconds) when the roughness of the detergent particles disappeared.

<Method for Measuring Specific Gravity of Foam of Anionic Surfactant Composition>
The specific gravity of the foam of the anionic surfactant composition obtained from the foaming machine is the composition of the anionic surfactant discharged from the foaming machine outlet after measuring the volume of an arbitrary container in advance using water at 20 ° C. Repeatedly tapping while gradually adding the foam of the product to the container, filling so that no voids are formed between the foam, and dividing the mass of the obtained foam by the volume of the container Thus, the temperature is measured at the time of foaming (temperature supplied to the foaming machine when a foaming machine is used). The specific gravity of the foam of the anionic surfactant composition after spraying can be recovered by collecting the sprayed anionic surfactant composition in a container such as a polyethylene bag or vat, and by the same method as described above at the temperature at the time of spraying. taking measurement. In addition, unless otherwise indicated in this specification, specific gravity is specific gravity with respect to the density of 20 degreeC water.

The present invention further discloses the following manufacturing method regarding the above-described embodiment.

<1> A method for producing a detergent particle group comprising a step of granulating a powder raw material for detergent using a container rotating mixer,
A method for producing a detergent particle group, in which a foam of an anionic surfactant composition is sprayed into the container rotary mixer using a multi-fluid nozzle to granulate the detergent powder raw material.

<2> The specific gravity of the foam of the anionic surfactant composition after spraying with a multi-fluid nozzle is 0.1 to 0.95, preferably 0.2 to 0.95, more preferably 0.2 to 0. .85, wherein the production method is <85>.
<3> The production method according to <1> or <2>, wherein the foam of the anionic surfactant composition is obtained by mixing a gas medium in the anionic surfactant composition. .
<4> The production method according to <3>, wherein the gas medium is mixed into the anionic surfactant composition using a foaming machine.
<5> The production method according to <3> or <4>, wherein the gas medium is air.
<6> The method according to any one of <1> to <5>, wherein the multi-fluid nozzle is a two-fluid nozzle.
<7> An anionic surfactant composition comprising the following components a) and b):
a) one or more anionic surfactants selected from the group consisting of salts of linear alkylbenzene sulfonic acids, salts of alkyl sulfates and salts of polyoxyethylene alkyl sulfates,
b) 25 to 70 parts by weight, preferably 30 to 65 parts by weight, more preferably 35 to 65 parts by weight of water based on 100 parts by weight of the component a)
The production method according to any one of the above items <1> to <6>, wherein the paste is a surfactant paste.

<8> The above <1> to <7>, wherein 20 to 100 parts by mass, preferably 25 to 90 parts by mass of the foam of the anionic surfactant composition is sprayed with respect to 100 parts by mass of the powder raw material for detergent. The manufacturing method of any one of these.
<9> The production method according to any one of <1> to <8>, wherein the detergent powder material is a water-soluble solid alkali inorganic substance and / or a water-soluble inorganic salt.
In the <10> detergent particle group, the content of the detergent powder raw material is 10% by mass or more, preferably 20% by mass or more, preferably 80% by mass or less, preferably 10 to 80% by mass, more preferably The production method according to any one of <1> to <9>, wherein the production method is 20 to 80% by mass.
<11> The production method according to any one of <1> to <10>, wherein the detergent powder raw material is sodium carbonate and / or sodium sulfate, preferably light ash.
<12> The anionic surfactant as the component a) is a salt of a linear alkylbenzene sulfonic acid having 10 to 18 carbon atoms, preferably 12 to 16 carbon atoms, 10 to 18 carbon atoms, preferably 12 to 16 carbon atoms. Any one of the above <7> to <11>, which is at least one selected from the group consisting of a salt of alkylsulfuric acid and a polyoxyethylene alkylsulfuric acid salt having 10 to 18 carbon atoms, preferably 12 to 16 carbon atoms The production method according to claim 1.
<13> The content of the anionic surfactant in the detergent particle group is 5% by mass or more, preferably 10% by mass or more, preferably 50% by mass or less, more preferably 40% by mass or less, preferably 5%. The production method according to any one of <1> to <12>, wherein the production amount is ˜50 mass%, more preferably 10 to 50 mass%, and still more preferably 10 to 40 mass%.
<14> The production method according to any one of <1> to <13>, wherein the container rotation type mixer is a drum type mixer or a pan type mixer.
<15> The specific gravity of the foam of the anionic surfactant composition is 0.1 to 0.9, preferably 0.1 to 0.8, more preferably 0.1 to 0.7. The production method according to any one of 1> to <14>.

<16> A multi-fluid nozzle is a nozzle for mixing a foam of an anionic surfactant composition and a gas for atomization, wherein [volume flow rate of foam of an anionic surfactant composition (cm ³ / min )] / [Flow rate of atomizing gas (L / min)] is in the range of 0.5 to 30 cm ³ / L, preferably 1 to 20 cm ³ / L, in the above <1> to <15> The manufacturing method of any one of Claims.
<17> Any one of the above <1> to <16>, wherein the obtained detergent particle group has a bulk density of 250 to 690 g / L, preferably 250 to 650 g / L, more preferably 300 to 600 g / L. The production method according to item.
<18> Granulation of the powder raw material for the detergent is performed under an operating condition in which the fluid number obtained from the following formula of the container rotary mixer is 0.005 to 1.0, preferably 0.01 to 0.6. The production method according to any one of <1> to <17>.
Fluid number: Fr = V ² / (R × g)
V: Circumferential speed [m / s]
R: Radius from the center of rotation to the circumference of the rotating object [m]
g: Gravity acceleration [m / s ² ]

Hereinafter, the present invention will be described in more detail based on examples and the like, but the present invention is not limited to such examples.

In the following examples and the like, the following raw materials were used unless otherwise specified. In addition,% of a composition in a table | surface means the mass%.
Sodium polyoxyethylene alkyl sulfate (70% pure, remaining water: C12 / C14 = 70/30 carbon number of alkyl group), “Emar 270J” manufactured by Kao
Sodium alkyl sulfate (pure content 66%, balance water; carbon number of alkyl group is C12 / C14 / C16 = 64/24/12 (mass%))
Sodium dodecylbenzenesulfonate (65% pure, balance water), Kao's “Neopelex G-65”
Light ash: average particle size 100 μm, manufactured by Central Glass Co., Ltd. Crushed light ash: pulverized light ash above to an average particle size of 10 μm Sodium sulfate: average particle size 200 μm, manufactured by Shikoku Kasei Kogyo Co., Ltd. "
Ground sodium sulfate: The above sodium sulfate ground to an average particle size of 22 μm. Zeolite: Average particle size of 3.5 μm, manufactured by Zeobuilder Co., Ltd. Sodium polyacrylate: manufactured by Kao Corp. Weight average molecular weight 10,000 (pure content 40%)
Polyethylene glycol: Kao Corporation weight average molecular weight 13000 (pure content 60%)

In the following examples and the like, a 75 L drum type mixer (φ40 cm × L60 cm) having a baffle plate was used as a container rotating mixer, tilted at 14 ° from the horizontal so that the bottom of the mixer was on the lower side. As the multi-fluid nozzle, one two-fluid nozzle (manufactured by Atmax Co., Ltd .: model number BN90) was used. The temperature of the foam of the anionic surfactant when supplying to the two-fluid nozzle was set to 60 ° C. The foam of the anionic surfactant composition was prepared using MDF0 (manufactured by Taiyo Kiko Co., Ltd.), which is a continuous foaming machine. The temperature of the composition when it was supplied to the foaming machine was 60 ° C.

Example 1 (Preparation of detergent particles)
100 parts by mass of sodium alkyl sulfate at 60 ° C. and 135 parts by mass of sodium dodecylbenzenesulfonate at 60 ° C. were mixed to prepare an anionic surfactant composition. The prepared anionic surfactant composition was a surfactant paste containing 52.8 parts by mass of water with respect to 100 parts by mass of the anionic surfactant. The viscosity of the paste at 60 ° C. was 1.7 Pa · s.

1.81 kg of light ash and 3.42 kg of pulverized sodium sulfate were added as a powder material for detergent into a drum mixer, and stirred for 30 seconds at a fluid number of 0.2. Thereafter, while continuing stirring, 1.55 kg of the foam of the anionic surfactant composition prepared by the MDF0 was added to the gas for atomization 80 L / min (volume flow rate of foam / for atomization) for 17 minutes. The gas was added through a two-fluid nozzle under a spraying condition of 5.3 cm ³ / L) and stirred for 1 minute after the addition. That is, 29.6 parts by mass of the foam was sprayed at 60 ° C. with respect to 100 parts by mass of the powder raw material for detergent. Thereafter, stirring was stopped, 0.22 kg of zeolite was added and stirring was performed for 1 minute under the same conditions as described above, and the resulting granulated product was discharged from a drum-type mixer to form a detergent particle group.

In addition, the flow rate of the mixed gas in the foaming machine was 0.50 L / min, and the specific gravity of the foam of the anionic surfactant composition obtained from the foaming machine was 0.20. Further, the specific gravity of the foam of the anionic surfactant composition after being sprayed by the two-fluid nozzle was 0.85, which was broken by the shearing force of the atomizing gas. Table 1 shows the composition and properties of the obtained detergent particles.

Example 2
Sodium alkyl sulfate was adjusted to 60 ° C. to obtain an anionic surfactant composition. The prepared anionic surfactant composition was a surfactant paste containing 51.52 parts by mass of water with respect to 100 parts by mass of the anionic surfactant. The viscosity of the paste at 60 ° C. was 1.4 Pa · s.

4.20 kg of pulverized sodium sulfate was added as a powder raw material for a detergent into a drum mixer and stirred for 30 seconds at a fluid number of 0.2. Thereafter, 2.80 kg of the foamed anionic surfactant composition thus prepared was added with a stirring time of 33 minutes, and the gas for atomization 80 L / min (volume flow rate of foam / flow rate of gas for atomization). Was added with a two-fluid nozzle under spraying conditions of 5.3 cm ³ / L) and stirred for 1 minute after the addition. That is, 66.7 parts by mass of the foam was sprayed at 60 ° C. with respect to 100 parts by mass of the powder raw material for detergent. Thereafter, stirring was stopped, and the resulting granulated product was discharged from a drum mixer to form a detergent particle group.

In addition, the flow rate of the mixed gas in the foaming machine was 0.50 L / min, and the specific gravity of the foam of the anionic surfactant composition obtained from the foaming machine was 0.20. In addition, the specific gravity of the foam of the anionic surfactant composition sprayed by the two-fluid nozzle was 0.85 when the foam was broken by the shearing force of the atomizing gas. Table 1 shows the composition and properties of the obtained detergent particles.

Example 3
Granulation is carried out under the same conditions as in Example 2 except that the flow rate of the atomization gas is 42 L / min (volume flow rate of foam / flow rate of atomization gas is 10.0 cm ³ / L). It was. The specific gravity of the foam of the anionic surfactant composition sprayed by the two-fluid nozzle was 0.68. Table 1 shows the composition and properties of the obtained detergent particles.

Example 4
Sodium alkyl sulfate was adjusted to 60 ° C. to obtain an anionic surfactant composition.

4.20 kg of light ash was added into a drum-type mixer as a powder raw material for detergent, and stirred for 30 seconds at a fluid number of 0.2. Thereafter, 2.80 kg of the foamed anionic surfactant composition thus prepared was added with a stirring time of 33 minutes, and the gas for atomization 80 L / min (volume flow rate of foam / flow rate of gas for atomization). Was added with a two-fluid nozzle under spraying conditions of 5.3 cm ³ / L) and stirred for 1 minute after the addition. That is, 66.7 parts by mass of the foam was sprayed at 60 ° C. with respect to 100 parts by mass of the powder raw material for detergent. Thereafter, stirring was stopped, and the resulting granulated product was discharged from a drum mixer to form a detergent particle group.

Example 5
The amount of gas mixture in the foaming machine is 0.10 L / min, and the specific gravity of the foam of the anionic surfactant composition obtained from the foaming machine is 0.58 (volume flow rate of foam / flow rate of atomization gas) Was granulated under the same conditions as in Example 4 except that it was 1.8 cm ³ / L). The specific gravity of the foam of the anionic surfactant composition sprayed by the two-fluid nozzle was similarly broken to 0.85. Table 1 shows the composition and properties of the obtained detergent particles.

Example 6
Sodium alkyl sulfate was adjusted to 60 ° C. to obtain an anionic surfactant composition. The prepared anionic surfactant composition was a surfactant paste containing 51.52 parts by mass of water with respect to 100 parts by mass of the anionic surfactant. The viscosity of the paste at 60 ° C. was 1.4 Pa · s.

4.20 kg of pulverized sodium sulfate was added as a powder raw material for a detergent into a drum mixer and stirred for 30 seconds at a fluid number of 0.2. Thereafter, 2.80 kg of the foam of the prepared anionic surfactant composition was added to the atomized gas 32 L / min (the volume flow rate of the foam / the gas for atomization) while the stirring was continued. Was added by a two-fluid nozzle under spraying conditions of 12.6 cm ³ / L) and stirred for 1 minute after the addition. That is, 66.7 parts by mass of the foam was sprayed at 60 ° C. with respect to 100 parts by mass of the powder raw material for detergent. Thereafter, stirring was stopped, and the resulting granulated product was discharged from a drum mixer to form a detergent particle group.

In addition, the flow rate of the mixed gas in the foaming machine was 0.50 L / min, and the specific gravity of the foam of the anionic surfactant composition obtained from the foaming machine was 0.20. In addition, the specific gravity of the foam of the anionic surfactant composition sprayed by the two-fluid nozzle was 0.44 when the foam was broken by the shearing force of the atomizing gas. Table 1 shows the composition and properties of the obtained detergent particles.

Example 7
Sodium alkyl sulfate was adjusted to 60 ° C. to obtain an anionic surfactant composition. The prepared anionic surfactant composition was a surfactant paste containing 51.52 parts by mass of water with respect to 100 parts by mass of the anionic surfactant. The viscosity of the paste at 60 ° C. was 1.4 Pa · s.

0.93 kg of pulverized light ash and 4.07 kg of pulverized sodium sulfate were added as a powder raw material for a detergent into a drum mixer and stirred for 30 seconds at a fluid number of 0.2. Thereafter, while the stirring was continued, 2.01 kg of the foamed anionic surfactant composition was added to an addition time of 22.6 minutes, atomization gas 29 L / min (volume flow rate of foam / gas for atomization). Was added with a two-fluid nozzle under spraying conditions of 15.2 cm ³ / L) and stirred for 1 minute after the addition. That is, 40.2 parts by mass of the foam was sprayed at 60 ° C. with respect to 100 parts by mass of the detergent powder raw material. Thereafter, stirring was stopped, and the resulting granulated product was discharged from a drum mixer to form a detergent particle group.

In addition, the flow rate of the mixed gas in the foaming machine was 0.50 L / min, and the specific gravity of the foam of the anionic surfactant composition obtained from the foaming machine was 0.20. In addition, the specific gravity of the foam of the anionic surfactant composition sprayed by the two-fluid nozzle was 0.39 as a result of breaking by the shearing force of the atomizing gas. Table 1 shows the composition and properties of the obtained detergent particles.

Example 8
Sodium alkyl sulfate was adjusted to 60 ° C. to obtain an anionic surfactant composition. The prepared anionic surfactant composition was a surfactant paste containing 51.52 parts by mass of water with respect to 100 parts by mass of the anionic surfactant. The viscosity of the paste at 60 ° C. was 1.4 Pa · s.

2.00 kg of pulverized light ash and 2.03 kg of pulverized sodium sulfate were added as a powder raw material for a detergent into a drum mixer and stirred for 30 seconds at a fluid number of 0.2. Thereafter, 2.24 kg of the foamed anionic surfactant composition thus prepared was added with a stirring time of 26.4 minutes, atomization gas 28 L / min (volume flow rate of foam / gas for atomization). Was added with a two-fluid nozzle under spraying conditions of 15.1 cm ³ / L) and stirred for 1 minute after the addition. That is, 55.7 parts by mass of the foam was sprayed at 60 ° C. with respect to 100 parts by mass of the powder raw material for detergent.

Subsequently, 0.19 kg of sodium polyacrylate at 60 ° C. and 0.025 kg of polyethylene glycol at 60 ° C. were added to the pot for feeding (with jacket, jacket temperature 60 ° C.), and the pressure was applied to the pot with air by 0.1 MPa, Opening the opening of the control valve at the pot outlet by 90 degrees, pumping and using a two-fluid nozzle (manufactured by Atmax Co., BN90) in a drum type mixer, spraying time 2.0 minutes, atomizing gas 80 L / min And stirred for 1 minute after the addition. Thereafter, stirring was stopped, 0.19 kg of zeolite was added and stirring was performed for 1 minute under the same conditions as described above, and the resulting granulated product was discharged from a drum type mixer to obtain a detergent particle group.

In addition, the flow rate of the mixed gas in the foaming machine was 0.50 L / min, and the specific gravity of the foam of the anionic surfactant composition obtained from the foaming machine was 0.20. In addition, the specific gravity of the foam of the anionic surfactant composition sprayed by the two-fluid nozzle was 0.36, which was broken by the shearing force of the atomizing gas. Table 1 shows the composition and properties of the obtained detergent particles.

Example 9
Sodium polyoxyethylene alkyl sulfate was adjusted to 60 ° C. to obtain an anionic surfactant composition. The prepared anionic surfactant composition was a surfactant paste containing 42.86 parts by mass of water with respect to 100 parts by mass of the anionic surfactant. The viscosity of the paste at 60 ° C. was 1.9 Pa · s.

4.67 kg of light ash was added as a powder raw material for a detergent into a drum mixer and stirred for 30 seconds at a fluid number of 0.2. Thereafter, with the stirring continued, 2.00 kg of the foamed anionic surfactant composition was added to the addition time 15.3 minutes, atomization gas 30 L / min (foam volume flow rate / atomization gas). Was added through a two-fluid nozzle under spraying conditions of 13.6 cm ³ / L) and stirred for 1 minute after the addition. That is, 42.83 parts by mass of the foam was sprayed at 60 ° C. with respect to 100 parts by mass of the detergent powder raw material. Thereafter, stirring was stopped, 0.33 kg of zeolite was added and stirring was performed for 1 minute under the same conditions as described above, and the resulting granulated product was discharged from a drum-type mixer to form a detergent particle group.

The flow rate of the mixed gas in the foaming machine was 0.29 L / min, and the specific gravity of the foam of the anionic surfactant composition obtained from the foaming machine was 0.32. In addition, the specific gravity of the foam of the anionic surfactant composition sprayed by the two-fluid nozzle was 0.67, which was broken by the shearing force of the atomizing gas. Table 1 shows the composition and properties of the obtained detergent particles.

Comparative Example 1
100 parts by mass of sodium alkyl sulfate at 60 ° C. and 135 parts by mass of sodium dodecylbenzenesulfonate at 60 ° C. were mixed to prepare an anionic surfactant composition.

1.81 kg of light ash and 3.42 kg of pulverized sodium sulfate were added as a powder material for detergent into a drum mixer, and stirred for 30 seconds at a fluid number of 0.2. Thereafter, with the stirring continued, 1.55 kg of the prepared anionic surfactant composition was added at an addition time of 17 minutes, atomization gas 80 L / min (volume flow rate of the composition / flow rate of atomization gas 1 0.1 cm ³ / L) was added with a two-fluid nozzle under a spraying condition, and stirred for 1 minute after the addition. That is, 29.64 parts by weight of the composition was sprayed at 60 ° C. with respect to 100 parts by weight of the detergent powder raw material. Thereafter, stirring was stopped, 0.22 kg of zeolite was added and stirring was performed for 1 minute under the same conditions as described above, and the resulting granulated product was discharged from a drum-type mixer to form a detergent particle group.

The specific gravity of the surfactant composition was 1.0, and the specific gravity after spraying with a two-fluid nozzle was 1.0. Table 1 shows the composition and properties of the obtained detergent particles.

Comparative Example 2
Sodium alkyl sulfate was adjusted to 60 ° C. to obtain an anionic surfactant composition.

4.20 kg of pulverized sodium sulfate was added as a powder raw material for a detergent into a drum mixer and stirred for 30 seconds at a fluid number of 0.2. Thereafter, with the stirring continued, 2.80 kg of the prepared anionic surfactant composition was added to an addition time of 33 minutes, atomization gas 80 L / min (volume flow rate of the composition / flow rate of atomization gas was 1). 0.1 cm ³ / L) was added with a two-fluid nozzle under a spraying condition, and stirred for 1 minute after the addition. That is, 66.7 parts by mass of the composition was sprayed at 60 ° C. with respect to 100 parts by mass of the powder raw material for detergent. Thereafter, stirring was stopped, and the resulting granulated product was discharged from a drum mixer to form a detergent particle group.

Comparative Example 3
Sodium alkyl sulfate was adjusted to 60 ° C. to obtain an anionic surfactant composition.

4.20 kg of pulverized sodium sulfate was added to a drum mixer as a powder material for detergent, and stirred for 30 seconds at a fluid number of 0.2. Thereafter, 2.80 kg of the prepared anionic surfactant composition foam was added with a two-fluid nozzle under a spraying condition of a gas for atomization of 0 L / min with an addition time of 33 minutes while stirring was continued. Stir for 1 minute. That is, 66.7 parts by mass of the foam was added at 60 ° C. with respect to 100 parts by mass of the detergent powder raw material. Thereafter, stirring was stopped, and the resulting granulated product was discharged from a drum mixer to form a detergent particle group.

In addition, the flow rate of the mixed gas in the foaming machine was 0.50 L / min, and the specific gravity of the foam of the anionic surfactant composition obtained from the foaming machine was 0.20. The specific gravity of the foam of the anionic surfactant composition added by the two-fluid nozzle was 0.20. This is considered to be the result of no bubble breakage due to the shearing force caused by the gas because the atomizing gas was not supplied. Table 1 shows the composition and properties of the obtained detergent particles.

Comparative Example 4
Sodium polyoxyethylene alkyl sulfate was adjusted to 60 ° C. to obtain an anionic surfactant composition. 4.33 kg of light ash was added into a drum mixer as a powder raw material for detergent, and stirred at a fluid number of 0.2 for 30 seconds. Thereafter, while continuing stirring, 2.33 kg of the prepared anionic surfactant composition was added for 18 minutes at an addition time of 80 L / min for atomization gas (volume flow rate of the composition / flow rate of atomization gas was 1). 0.5 cm ³ / L) was added by a two-fluid nozzle under the spraying condition, and stirred for 1 minute after the addition. That is, 53.8 parts by mass of the composition was sprayed at 60 ° C. with respect to 100 parts by mass of the powder raw material for detergent. Thereafter, stirring was stopped, 0.66 kg of zeolite was added, and stirring was performed for 1 minute under the same conditions as described above, and the resulting granulated product was discharged from a drum mixer to form a detergent particle group.

The specific gravity of the surfactant composition was 1.08, and the specific gravity after spraying with a two-fluid nozzle was 1.08. Table 1 shows the composition and properties of the obtained detergent particles.

The bulk of the detergent particles obtained in Examples 1 to 9 was 444 to 682 g / L. In addition, the granulation yield was 96% or more, and a medium and low bulk density detergent particle group was obtained with good yield. Furthermore, even in the case of a composition containing a large amount of sodium sulfate that falls into a category with a large specific gravity among the powder raw materials for detergents, a detergent particle group having a medium to low bulk density could be obtained with a high yield.

On the other hand, Comparative Examples 1, 2, and 4 became detergent particle groups with higher bulk density (715 g / L or more) than the Examples. This is presumably because the foam of the anionic surfactant composition having a low specific gravity was not provided with the effect of the foam because the foam of the anionic surfactant composition was not used.

For Comparative Example 3, the granulation yield was lower (60.6%) than in the Examples. This is because the foam of the anionic surfactant composition is used, but the atomization gas is set to 0 L / min, that is, the foam is sprayed substantially through one fluid nozzle. It is considered that the high dispersion of the body was not achieved and the formation of coarse particles was caused by the adhesiveness of the foam. Further, Comparative Example 3 was a detergent particle group having a higher bulk density (743 g / L) than the Examples. This is because the foam of the anionic surfactant composition was supplied as a large liquid mass, and as a result, the time required for hydration and dissolution of the detergent powder raw material in contact with the detergent powder raw material, It is also considered that the time for cooling by the detergent powder raw material increased as compared with the case of fine droplets, the foam was hard to solidify, and foam foaming during granulation was more likely to occur.

Furthermore, when Example 1 and Comparative Example 1 having the same composition were compared, the dissolution rate was improved for 60 seconds, and the roughness disappearance time was shortened. As can be seen from the fact that the bulk density in Example 1 was lower than that in Comparative Example 1, it is considered that the use of the foam increased the number of voids in the particles and facilitated dissolution. . Furthermore, as shown by the values of the coarse particle ratio and fine powder ratio, the particle size distribution became sharp and the fluidity was improved.

According to the present invention, a medium and low bulk density detergent particle group can be produced with high yield by a method that does not use spray drying. Such a detergent particle group can be preferably used as a detergent composition for various uses such as clothing, or as one component of such a detergent composition.

Claims

A method for producing detergent particles having a step of granulating a powder raw material for detergent using a container rotary mixer,
A method for producing a detergent particle group, in which a foam of an anionic surfactant composition is sprayed into the container rotary mixer using a multi-fluid nozzle to granulate the detergent powder raw material.
2. The production method according to claim 1, wherein the specific gravity of the foam of the anionic surfactant composition after spraying with a multi-fluid nozzle is 0.1 to 0.95.
The production method according to claim 1 or 2, wherein the foam of the anionic surfactant composition is obtained by mixing a gas medium in the anionic surfactant composition.
The production method according to claim 3, wherein mixing of the gas medium into the anionic surfactant composition is performed using a foaming machine.
The manufacturing method according to claim 3 or 4, wherein the gas medium is air.
The manufacturing method according to any one of claims 1 to 5, wherein the multi-fluid nozzle is a two-fluid nozzle.
The anionic surfactant composition comprises the following components a) and b):
a) one or more anionic surfactants selected from the group consisting of salts of linear alkylbenzene sulfonic acids, salts of alkyl sulfates and salts of polyoxyethylene alkyl sulfates,
b) 25 to 70 parts by weight of water with respect to 100 parts by weight of component a) above;
The production method according to any one of claims 1 to 6, which is a surfactant paste containing
The production method according to any one of claims 1 to 7, wherein a foam of 20 to 100 parts by mass of an anionic surfactant composition is sprayed with respect to 100 parts by mass of the powder raw material for detergent.
The production method according to any one of claims 1 to 8, wherein the content of the anionic surfactant in the detergent particle group is 5 to 50% by mass.
The production method according to any one of claims 1 to 9, wherein the content of the detergent powder raw material is 10 to 80% by mass in the detergent particle group.
The production method according to any one of claims 1 to 10, wherein the powder raw material for the detergent is a water-soluble solid alkali inorganic substance and / or a water-soluble inorganic salt.