JP2012255146A - Method for producing detergent particle group - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for producing a detergent particle group containing an anionic surfactant and having excellent solubility in water at low temperature in a method not involving spray drying.SOLUTION: The method for producing the detergent particle group including a surfactant paste mixing step includes adding a surfactant paste containing (a) an anionic surfactant, (c) an alkyl glyceryl ether and (b) water to a powdery detergent raw material by using a multi-fluid nozzle and mixing them with a rotating vessel granulator.

Description

  The present invention relates to a surfactant paste containing an anionic surfactant, alkyl glyceryl ether and water, a container rotating granulator, and a method for producing detergent particles using a multi-fluid nozzle. Furthermore, this invention relates to the detergent composition formed by containing this detergent particle group.

  In recent years, the powder detergent composition and its production method have been required to be economical and environmentally friendly.

  With respect to powder detergents containing an anionic surfactant such as an alkyl sulfate salt as a surfactant, various disclosures have been made so far for the purpose of improving high cleaning activity and environmental friendliness. Such anionic surfactants are generally known to have low skin irritation and good biodegradability.

  For example, from the viewpoint of economy and environmental friendliness, as a production method not using spray drying, a method for producing a detergent composition using an anionic surfactant by a non-spray drying method is disclosed. 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 more easily obtain a group of detergent particles having a required particle size. Further, in these patent documents, no consideration is given to solubility in low-temperature water.

Japanese National Patent Publication No. 10-500716 Japanese National Patent Publication No. 10-506141

  Accordingly, an object of the present invention is to provide a method for producing a group of detergent particles containing an anionic surfactant and having good solubility in low-temperature water by a method that does not involve spray drying.

That is, the gist of the present invention is as follows.
[1]
In powder detergent raw materials, the following a) component, c) component and b) component:
a) Anionic surfactant
c) Alkyl glyceryl ether
b) A method for producing detergent particles including a surfactant paste mixing step, in which a surfactant paste containing water is added using a multi-fluid nozzle and mixed by a container rotating granulator;
[2]
Detergent particles obtained by the production method according to [1] above; and [3]
A detergent composition comprising a detergent particle group obtained by the production method according to the above [1];
It is about.

  By using the production method of the present invention, it is possible to produce a detergent particle group having excellent solubility in low-temperature water and having a sharp particle size distribution with high yield. Sharpening the particle size distribution not only improves the appearance, but also has good fluidity, and as a result, it is possible to efficiently obtain a detergent with excellent productivity.

  The method for producing detergent particles of the present invention is a method for producing detergent particles having a step of mixing a surfactant paste containing an anionic surfactant, an alkyl glyceryl ether and water, and a powder detergent raw material. In mixing, one feature is that a container rotating granulator is used and the surfactant paste is added using a multi-fluid nozzle such as a two-fluid nozzle.

  In general, granulation using a container rotating granulator makes it possible to uniformly flow the powder in the granulator, and further, because of the mixing mechanism that involves lifting of particles by rotation and sliding and dropping by its own weight, Since the shearing force applied to the powder is suppressed, this is a non-consolidated granulation method. In addition, since the paste containing an anionic surfactant does not proceed with granulation unless the adhesiveness when contacting with the powder is strong, it is necessary to develop the adhesiveness when contacting with the powder. . When such a paste is supplied to a container rotary granulator by a one-fluid nozzle or pipe, which is a general supply method, the supplied liquid component is difficult to disperse uniformly in the mixer and is locally generated. It was found that large particles are likely to form coarse particles.

  Therefore, by using a multi-fluid nozzle such as a two-fluid nozzle, a container is formed by spraying a paste further containing an anionic surfactant that exhibits adhesiveness when contacted with powder and an alkyl glyceryl ether. Surprisingly, it was found that uniform granulation was possible while suppressing the formation of coarse particles. This is because such a paste is made into fine droplets in advance using a multi-fluid nozzle, so that high dispersion of such paste can be achieved even in a container rotary granulator, and coarse particles are formed. This is probably because a large liquid mass is not generated. Therefore, it is also one of the features of the present invention that such a paste that develops adhesiveness when in contact with the powder is added to the container rotating granulator using a multi-fluid nozzle.

  Thus, in the present invention, by using a container rotary granulator and a multi-fluid nozzle in combination, it is possible to obtain a detergent particle group having a sharp particle size distribution, which is unpredictable when used alone. The effect which can be manufactured well is produced.

  As a hypothesis of the mechanism by which particles with a sharp particle size distribution can be obtained in high yield, uniform particles with suppressed shearing force applied to the powder can be obtained by using a container rotating granulator, and This is considered to be due to a synergistic effect that the droplets are finely dispersed and highly dispersed by the multi-fluid nozzle, and thus aggregation caused by the adhesiveness of the surfactant paste containing the anionic surfactant can be suppressed.

  However, when stirring or mixing is performed using a container rotating granulator, there is a problem that a liquid component (a surfactant paste in this specification) is difficult to be uniformly dispersed in the granulator. Therefore, for example, a method of uniformly dispersing the liquid component by considering a liquid component supply method can be considered. For example, as a method of uniformly dispersing the liquid component, a method of miniaturizing the liquid component using a multi-fluid nozzle such as a two-fluid nozzle can be considered. However, the idea of using a multi-fluid nozzle to refine a highly viscous surfactant paste is unlikely to occur even by those skilled in the art.

  As a mixing mode in the production method of the present invention, a container rotating granulator is used, and a surfactant paste containing an anionic surfactant, alkyl glyceryl ether and water is sprayed using a multi-fluid nozzle. Although it will not specifically limit if it is an aspect, 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, a builder and the like, 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.

1. Powder detergent raw material An essential component in the present invention is a powder detergent raw material. Specific examples include 1) alkaline agents, 2) water-soluble substances, and 3) clay minerals. As these components 1) to 3), an alkali agent, a water-soluble substance, and a clay mineral may be used alone, or a plurality of components may be mixed and used. From the viewpoint of granulation, the average particle size of the powder detergent raw material is preferably 10 to 250 μm, more preferably 50 to 200 μm, and still more preferably 80 to 200 μm.

  The average particle size of the alkali agent, water-soluble substance, and clay mineral is not particularly limited. However, when the surfactant paste is highly blended, it may be used after pulverizing to 1 to 50 μm from the viewpoint of improving the yield. Good.

  Examples of the alkali agent include those used as an alkali agent in ordinary detergent compositions, and examples include sodium carbonate (for example, light ash or dense ash), sodium hydrogen carbonate, sodium silicate, potassium carbonate, calcium carbonate and the like. . Light ash is preferable from the viewpoint of ease of handling and availability. These may be used alone or in combination of two or more.

  When light ash is used as the powder detergent raw material, the ability to carry the surfactant can be further improved by adjusting the temperature during baking soda baking. From the viewpoint of supporting ability, the firing temperature is preferably 120 to 250 ° C, preferably 150 to 220 ° C, and more preferably 150 to 200 ° C.

  Examples of water-soluble substances include powders used in ordinary detergent compositions such as mirabilite and sodium tripolyphosphate, and porous powders prepared by drying these hydrates.

  Examples of the clay mineral include clay minerals used in ordinary detergent compositions. As a powder detergent raw material, when using a clay mineral and the said other raw material together, those mixtures will be granulated. When mixed with the surfactant paste, a part of the powder detergent raw material is dissolved by the water contained in the paste, and the caking property produced thereby or the caking property of clay mineral is used for granulation.

  When mixing powder detergent raw material powder and surfactant paste, powder raw materials other than the powder detergent raw material may be added as desired. 0-150 mass parts is preferable, 0-100 mass parts is more preferable, and 0-50 mass parts is more preferable. Examples of the powder raw material include crystalline silicates such as aluminosilicate and prefeed (manufactured by Tokuyama Siltec Co., Ltd.). When using such a powder raw material, the content of the powder raw material in the detergent particle group is preferably 0.1% by mass or more from the viewpoint of improving fluidity, suppressing smearing and caking, and improving cleaning power, 1 mass% or more is more preferable, 3 mass% or more is more preferable, 40 mass% or less is preferable from a viewpoint of rinse property and solubility, 30 mass% or less is more preferable, 20 mass% or less is further more preferable, 10 mass% The following is even more preferable.

  From the viewpoint of availability and the performance of the resulting detergent particle group, preferred examples of the powder detergent raw material include those containing light ash and / or sodium sulfate.

2. Surfactant paste An essential component in the present invention is a surfactant paste. In the present invention, by adding a surfactant paste to a powder detergent raw material and using a container rotating granulator, the powder detergent raw material is granulated to produce a detergent particle group.

[Composition of surfactant paste]
The anionic surfactant (in this specification, a) component in the surfactant paste used for this invention is described. In general, those used for clothing detergents, vegetable / dishwashing detergents, hair / skin cleaners, and the like can be used. For example, alkyl sulfate ester salt, polyoxyethylene alkyl sulfate ester salt, α-sulfo fatty acid ester salt, α-olefin sulfonate, alkyl or hydroxyalkyl ether carboxylate, N-acylated taurine, N-acylated methyl taurine N-acylated glycine, N-acylated aspartic acid, N-acylated sarcosine, N-acylated glutamic acid, higher fatty acid salt, alkylbenzene sulfonate, alkyl sulfate, monoalkyl phosphate ester salt, alkylamide ether sulfate Examples include ester salts, fatty acid monoglyceride sulfates, and alkyliminodicarboxylates. From the viewpoint of improving the solubility of the detergent particles in low-temperature water, one or more selected from the group consisting of alkyl sulfates, polyoxyethylene alkyl sulfates and alkylbenzene sulfonates are preferred.

In addition to the solubility of the detergent particles in low-temperature water, from the viewpoint of producing detergent particles having a sharp particle size distribution, the anionic surfactant in the surfactant paste used in the present invention is represented by the formula ( 1): An alkyl sulfate ester salt represented by R—O—SO ₃ M is more preferable. In the formula (1), R is an alkyl group or alkenyl group having 10 to 18 carbon atoms, preferably 12 to 16 carbon atoms, M is an alkali metal atom such as Na or K, ammonia or monoethanolamine, diethanolamine or the like. It is an amine. From the viewpoint of improving the detergency of the detergent composition, M and Na are preferably K. Specific examples of R include decyl group, lauryl group, myristyl group, cetyl group and the like.

The alkyl glyceryl ether used in the present invention (herein referred to as component c). ) Is the following general formula (3):
R ¹ —OCH ₂ —CHOH—CH ₂ OH (3)
(Wherein R ¹ represents a linear or branched alkyl group or alkenyl group having 1 to 24 carbon atoms, or a cycloalkyl group having 3 to 8 carbon atoms).

In the general formula (3), R ¹ is a linear or branched alkyl or alkenyl group having 1 to 24 carbon atoms, preferably 3 to 24 carbon atoms, or preferably a cycloalkyl group having 3 to 8 carbon atoms. . From the viewpoint of improving the solubility of the detergent particles in low-temperature water, a linear or branched alkyl group having 6 to 18 carbon atoms is more preferable, and an alkyl group having 8 to 12 carbon atoms is more preferable. As the alkyl group, a branched chain is more preferable.

Specifically, R ¹ includes hexyl, heptyl, octyl, nonyl, decyl, undecyl, dodecyl, tridecyl, tetradecyl, pentadecyl, hexadecyl, heptadecyl, octadecyl, etc. Linear alkyl groups, 2-ethylhexyl groups, 2-methylheptyl groups, 2-methylnonyl groups, 2-octyldecyl groups, 3,5,5-trimethylhexyl groups, isodecyl groups, isostearyl groups, and the like, Examples include alkenyl groups such as oleyl group.

  As the blending amount of the alkyl glyceryl ether of component c) in this step, from the viewpoint of improving the solubility of the detergent particles in low-temperature water, with respect to 100 parts by mass of the anionic surfactant in the surfactant paste 10-40 mass parts is preferable, 15-40 mass parts is more preferable, 15-38 mass parts is further more preferable.

  In addition to a predetermined amount of anionic surfactant, a predetermined amount of alkyl glyceryl ether, and a predetermined amount of water, the surfactant paste may contain components other than these components as required. .

[Physical properties of surfactant paste]
The viscosity of the surfactant paste is preferably 10 Pa · s or less, more preferably 5 Pa · s or less, preferably 0 or less, preferably from the viewpoint of handleability in production in the use temperature range of the surfactant paste. It is 0.5 Pa · s or more, more preferably 1 Pa · s or less, and 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 viscosity of the surfactant paste varies greatly depending on its water content. For example, a surfactant paste can be prepared by neutralizing the acid precursor of component a) with an alkali compound, but at this time, the water content of the alkali compound used is adjusted to obtain a desired moisture content. It is preferable to prepare a surfactant paste having a desired viscosity. When the surfactant paste contains 25 to 70 parts by mass of water with respect to 100 parts by mass of component a), the surfactant paste falls within this range in the present invention from the viewpoint that the viscosity is lowered and handling is easy. It is preferable to use a liquid whose water content is adjusted. The range of the amount of water in the surfactant paste is 25 to 70 parts by mass, preferably 30 to 65 parts by mass, more preferably 35 to 65 parts by mass with respect to 100 parts by mass of component a) from the viewpoint of handling. In addition, the water content in the surfactant paste is preferably 15 to 40% by mass, more preferably 20 to 37% by mass, and still more preferably 25 to 35% by mass from the viewpoint of handling.

  The method for preparing the surfactant paste is not particularly limited, and a known method can be used. In addition, since the acid precursor of component a) is very unstable and easily decomposes, it is 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. In use, the surfactant paste may be used after raising the temperature as necessary.

  Moreover, it is preferable that this anionic surfactant paste obtained has excess alkalinity from a viewpoint of suppressing decomposition | disassembly.

  In addition, to the surfactant paste, a) 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, added during the neutralization reaction PH buffering agents, depigmenting agents and the like that may be used may be contained.

  The content of the component a) in the detergent particle group obtained in the present invention is preferably in the range of 10 to 55% by mass, from 10 to 45% by mass, from the viewpoint of detergency and solubility in low-temperature water. Is more preferable, 15-40 mass% is further more preferable, and 15-35 mass% is still more preferable. In addition, the content of the component c) in the detergent particle group obtained in the present invention is preferably in the range of 1 to 22% by mass, more preferably 1 to 18% by mass, from the viewpoint of solubility in low-temperature water. 1.5 to 15% by mass is more preferable, 2 to 13% by mass is even more preferable, and the content of the powder detergent raw material is preferably 30 to 80% by mass and more preferably 40 to 75% by mass from the viewpoint of detergency. Preferably, 45 to 70% by mass is even more preferable.

  In the surfactant paste, the component a) can be used alone as the surfactant, but the following surfactant can also be used in combination. When used in combination, it may be mixed with the surfactant paste containing the component a) in advance, or may be added separately. In addition, when using the following surfactant together, the following surfactant is preferably 1 to 70 parts by weight, more preferably 2 to 50 parts by weight, and further preferably 3 to 30 parts with respect to 100 parts by weight of component a). It contains 5 to 15 parts by mass, still more preferably 5 to 15 parts by mass. Moreover, when using the following surfactant together, content of a) component in surfactant paste becomes like this. Preferably it is 40-80 mass%, More preferably, it is 45-75 mass%, More preferably, it is 50-70 mass%. It is.

  For example, nonionic surfactants can be mixed or used separately. In the case of using a nonionic surfactant having a melting point of 30 ° C. or lower, a water-soluble nonionic organic compound having a melting point of 45 to 100 ° C. and a molecular weight of 1,000 to 30,000, which has an effect of increasing the melting point of the surfactant. (Hereinafter, referred to as a melting point raising agent) or an aqueous solution thereof is preferably used in combination. Examples of the melting point raising agent that can be used in the present invention include polyethylene glycol, polypropylene glycol, polyoxyethylene alkyl ether, and pluronic-type nonionic surfactant. Further, amphoteric surfactants and cationic surfactants can be used in combination for the purpose.

  For example, anionic surfactants other than component a) can be mixed or used separately. Examples of such anionic surfactants include polyoxyethylene alkyl ether sulfates, alkylbenzene sulfonates, and α-sulfo fatty acids. Examples include ester salts and secondary alkane sulfonates. Further, from the viewpoint of improving the dispersibility of the detergent particles in low-temperature water, an anionic surfactant such as polyoxyethylene alkyl ether sulfate or alkylbenzene sulfonate is preferably 0 to 10 mass in the detergent particles. %, More preferably 0 to 5% by mass, still more preferably 0 to 3% by mass. Further, from the viewpoint of improving detergency, it is preferably 0.1% by mass or more, more preferably 1% by mass or more, further preferably 3% by mass or more, and from the viewpoint of improving detergent yield, 10% by mass or less is preferable, and 8% by mass. % Or less is more preferable, and 5 mass% or less is more preferable.

  Furthermore, in order to obtain an antifoaming effect, a fatty acid salt can be used in combination.

  Although it does not specifically limit as a nonionic surfactant, From a viewpoint of detergency, the polyoxyalkylene alkyl ether which added 6-22 mol of alkylene oxides to C10-C14 alcohol is preferable, for example.

  The content of the nonionic surfactant in the detergent particle group is preferably 0 to 10 mass in the detergent particle group from the viewpoints of improvement in detergency, improvement in caking resistance, and suppression of waste during powdering. %, More preferably, it is 0-5 mass%, More preferably, it is 0-3 mass%. Further, from the viewpoint of improving detergency, it is preferably 0.1% by mass or more, more preferably 1% by mass or more, further preferably 3% by mass or more, and from the viewpoint of improving detergent yield, 10% by mass or less is preferable, and 8% by mass. % Or less is more preferable, and 5 mass% or less is more preferable.

3. Polymer In addition, the detergent particles in the present invention include a water-soluble cellulose derivative, a saccharide and carboxylic acid polymer, an inorganic polymer such as an amorphous silicate, etc. from the viewpoint of a detergency and a binder effect for granulation A salt of acrylic acid-maleic acid copolymer and polyacrylate are more preferable. The salt is preferably a sodium salt, potassium salt or ammonium salt. In addition, as a weight average molecular weight of a carboxylic acid-type polymer, 1000-100000 are preferable and 2000-80000 are more preferable.

4). Other Components In the detergent particle group in the present invention, even if it is a substance other than those listed in the above 1 to 3, it can be appropriately blended as necessary. There is no particular limitation on the timing of addition of such other components.

・ Chelating agent (metal sequestering agent)
It can mix | blend in order to suppress the washing | cleaning action inhibition by a metal ion. The water-soluble chelating agent is not particularly limited as long as it is a substance that retains sequestering ability, but crystalline silicate, tripolyphosphate, orthophosphate, pyrophosphate, and the like can be used. The water-insoluble chelating agent preferably has an average particle diameter of 0.1 to 20 μm from the viewpoint of dispersibility in water, and examples thereof include crystalline aluminosilicates, such as A-type zeolite, P-type zeolite, X-type zeolite can be used.

-Water-soluble inorganic salt It is preferable to add a water-soluble inorganic salt in order to increase the ionic strength of the washing liquid and improve the effect of washing sebum dirt.

・ Water-insoluble excipient No particular limitation is imposed on the substance as long as it has good dispersibility in water and does not adversely affect detergency. From the viewpoint of dispersibility in water, primary particles having an average particle diameter of 0.1 to 20 μm are preferable.

-Other auxiliary components Fluorescent dyes, pigments, dyes, etc. are listed.

  In addition, the measurement of the average particle diameter of the said component can be measured by the method as described in the measuring method of the below-mentioned physical property.

<Production method of detergent particles>
The detergent particle group production method of the present invention is a method including a step of adding and mixing a surfactant paste to a powder detergent raw material in the following surfactant paste mixing step, and the detergent particle group is prepared through such a step. Is done.

1. Surfactant paste mixing step Add a surfactant paste containing an anionic surfactant, alkyl glyceryl ether and water to the powder of the powder detergent raw material, mix these with a container rotating granulator, and then use the detergent particles. It is a process of preparing a group.

  The amount of the surfactant paste added in this step is preferably 25 to 200 parts by weight, more preferably 25 to 180 parts by weight, still more preferably 25 to 160 parts by weight, with respect to 100 parts by weight of the powder detergent raw material. 25-100 mass parts is still more preferable, 30-90 mass parts is especially preferable, and 35-85 mass parts is especially more preferable. From the viewpoint of detergency, it is preferably 25 parts by mass or more, and from the viewpoint of detergent yield and solubility, it is preferably 200 parts by mass or less, more preferably 180 parts by mass or less, and further 160 parts by mass or less. Preferably, 100 parts by mass or less is even more preferable.

  The container rotating granulator used in this step may be an apparatus that gives strong shearing to the granules and does not cause large compaction. For example, even in a vertical or horizontal granulator originally provided with a main wing and a crushing blade capable of giving a high shearing force, the granule of the present invention can be controlled by setting the number of rotations and the fluid number described below to a low level to suppress compaction. Can be used for manufacturing. That is, the container rotating granulator in the present specification includes a granulator capable of operating with a reduced shearing force by setting operating conditions, etc., even if it is a granulator capable of giving a high shearing force to granules. Machines are also included.

  As the container rotating granulator, a pan granulator or a drum granulator in which granulation proceeds by rotation of the main body is preferable from the viewpoint of ease of granulation and improvement of supporting ability. These apparatuses can be used in both batch and continuous processes. From the viewpoint of powder mixing property and solid-liquid mixing property, it is preferable to provide a baffle plate for assisting mixing in the pan or drum.

  In addition, in order to use as a container rotating granulator, the powder can be made to flow uniformly, and from the viewpoint of securing a mixing mechanism that involves lifting of particles by rotation and sliding / falling by its own weight, The fluid number of the granulator defined by the formula is preferably set to 1.0 or less, more preferably 0.8 or less, still more preferably 0.6 or less, and even more preferably 0.4 or less.

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 ]

  From the viewpoint of uniformly adding the surfactant paste to the mixed powder, it is preferable to set the fluid number of the granulator to 0.001 or more, more preferably 0.005 or more, still more preferably 0.01 or more, 0 .05 or more is even more preferable.

  In a vertical or horizontal granulator equipped with main wings and crushing wings, V and R use the value of the main shaft, and a bread granulator or a drum granulator in which granulation proceeds by rotation of the body barrel. In this case, the values of the body trunk are used for V and R. In a bread granulator equipped with a crushing blade, V and R use values of the crushing blade.

  Although the rotation time of a granulator is not specifically limited, For example, 0 to 10 minutes are preferable after surfactant paste addition.

  In the present invention, the surfactant paste is uniformly dispersed and added, in addition to improving the solubility of the detergent particles in low-temperature water, from the viewpoint of producing detergent particles having a sharp particle size distribution, preferable. As a method therefor, there is a method of miniaturizing the surfactant paste using a multi-fluid nozzle.

  A multi-fluid nozzle is a nozzle that circulates a liquid component and atomizing gas (air, nitrogen, etc.) to the vicinity of the tip of the nozzle through an independent flow path, and mixes and atomizes the two-fluid nozzle, three-fluid nozzle, A four-fluid nozzle or the like can be used. Further, the mixing part of the liquid component and the atomizing gas may be either an internal mixing type that mixes within the nozzle tip or an external mixing type that mixes outside the nozzle tip.

  In the present invention, the surfactant paste is preferably added in the form of fine droplets using a multi-fluid nozzle, and more preferably a two-fluid nozzle. As such a multi-fluid nozzle, for example, 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., Spraying Systems Japan Co., Ltd. , Manufactured by Kyoritsu Alloy Manufacturing Co., Ltd., manufactured by Atmax Co., Ltd., and the like, and external mixed type two fluid nozzles manufactured by Fujisaki Electric Co., Ltd. and the like.

  When using a two-fluid nozzle, for example, it is preferable to supply the paste under the following conditions. For example, the air spray pressure for atomization is preferably 0.05 to 0.7 MPa.

  In the present invention, it is preferable to use an external mixing type two-fluid nozzle from the viewpoint of miniaturizing droplets of the high-viscosity surfactant paste used in the present invention and preventing clogging of the nozzle tip.

  As a result of earnestly examining the influence of the difference in droplet size on the yield and coarse particle amount of the resulting detergent particles, the average droplet size of the paste is 1 to 300 μm. 1 to 200 μm is more preferable, and 1 to 150 μm is more preferable.

  When it is desired to increase the addition speed of the paste, it is also effective to use a plurality of these multi-fluid nozzles and increase the addition speed while maintaining finer droplets.

  By using such a method, even a high-viscosity paste can be uniformly dispersed, and the yield can be improved and a detergent particle group having a sharp particle size distribution can be obtained.

  In addition, the average particle diameter of the droplet diameter of the surfactant paste is calculated on a volume basis, and is a value measured using a laser diffraction particle size distribution analyzer: Spray Tech (manufactured by Malvern).

<Physical properties of detergent particles>
A detergent particle group having predetermined characteristics can be obtained by the production method of the present invention. The detergent particle group obtained by the production method of the present invention is also included in the present invention. Preferred physical properties of the detergent particles according to the present invention are as follows.

  The bulk density is preferably 400 g / L or more, more preferably 450 to 1000 g / L, still more preferably 450 to 950 g / L, and more preferably 500 to 900 g / L. As an average particle diameter, Preferably it is 150-800 micrometers, More preferably, it is 180-700 micrometers, More preferably, it is 200-500 micrometers. If necessary, the obtained detergent particles may be sieved or pulverized.

  In addition, the said bulk density and an average particle diameter can be measured by the method as described in the measuring method of the below-mentioned physical property.

  The water content of the detergent particles in the present invention is preferably smaller from the viewpoint of high blending of component a). Specifically, when the moisture content of the detergent particle group is measured with an infrared moisture meter, the moisture content is preferably 20% by mass or less, more preferably 15% by mass or less, still more preferably 10% by mass or less, and further preferably 5% by mass. The following is more preferable.

The dissolution rate of the detergent particles for 60 seconds is calculated by the following method.
1 liter of hard water (Ca / Mg molar ratio 7/3) corresponding to 71.2 mg CaCO ₃ / liter cooled to 5 ° C. is a 1 liter beaker (inner diameter 105 mm, height 150 mm cylindrical type, for example, manufactured by Iwaki Glass Co., Ltd. 1 In a state where the water temperature of 5 ° C. is kept constant in a water bath, the stirring bar (length: 35 mm, diameter: 8 mm, for example, model: manufactured by ADVANTEC, trade name: Teflon (registered trademark)) In SA (round thin type), stirring is performed at a rotational speed (800 r / m) at which the spiral depth 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 charging, the detergent particle group dispersion in the beaker is filtered through a standard sieve (diameter: 100 mm) having an opening of 74 μm as defined in JISZ8801 of known mass, and the water-containing detergent particle groups remaining on the sieve are collected together with the sieve. Collect in a collection 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 the detergent particles is dried together with a sieve in an electric dryer heated to 105 ° C. for 1 hour, and then cooled for 30 minutes in a desiccator (25 ° C.) containing silica gel. After cooling, the total mass of the dissolved residue of the dried detergent particle group, the sieve, and the collection container is measured, and the dissolution rate (%) of the detergent particle group is calculated by Equation (4).

Dissolution rate (%) = {1- (T / S)} × 100 (4)
S: input mass of detergent particles (g)
T: Dry mass (g) of the dissolved residue of the detergent particles remaining on the sieve when the dispersion obtained under the above stirring conditions is applied to the sieve.

  It can be said that the higher the dissolution rate of the detergent particle group under such conditions is for 60 seconds, the better the detergent particle group is at low temperature solubility. In the present specification, the preferable dissolution rate of the detergent particles for 60 seconds is 70% or more, more preferably 80% or more, and still more preferably 85% or more.

  The suitable manufacturing method which obtains a detergent particle group may further include a liquid detergent raw material oil absorption process or a surface modification process, or a drying process as needed.

2. Arbitrary manufacturing process The detergent particle group obtained by this invention may contain the following process further.
Liquid detergent raw material oil absorption step: This is a step of mixing the detergent particles obtained in the surfactant paste mixing step with liquid detergent raw materials such as the nonionic surfactant and the polymer.
Surface modification step: This is a step of modifying the surface of the detergent particles obtained in the surfactant paste mixing step or the liquid detergent raw material oil absorption step with a surface coating agent such as aluminosilicate. However, crushing may proceed simultaneously in the surface modification step.
Drying step: A step of drying the detergent particles obtained in the surfactant paste mixing step, the liquid detergent raw material oil absorption step or the surface modification step.

<Detergent composition>
The detergent composition of the present invention is a composition comprising the above-described detergent particle group, and further contains detergent components (for example, builder granules, fluorescent dyes, enzymes, perfumes, odorants, etc.) separately added to the detergent particle group. A foaming agent, a bleaching agent, a bleaching activator, etc.).

  The content of the detergent particles in the detergent composition is preferably 50% by mass or more, more preferably 60% by mass or more, further preferably 70% by mass or more, and more preferably 80 to 100% by mass from the viewpoint of detergency.

  The content of detergent components other than the detergent particle group in the detergent composition is preferably 50% by mass or less, more preferably 40% by mass or less, still more preferably 30% by mass or less, and even more preferably 20% by mass or less.

<Production method of detergent composition>
The method for producing the detergent composition is not particularly limited, and examples thereof include a method of mixing the detergent particle group and a separately added detergent component. Since the detergent composition thus obtained contains detergent particles highly blended with the component a), a sufficient cleaning effect can be achieved even with a small amount. The use of such a detergent composition is not particularly limited as long as it is a use using a powder detergent, and examples thereof include a powder detergent for clothing and a detergent for automatic tableware.

<Method of measuring physical properties>
1. Bulk density The bulk density is measured by a method defined by JIS K 3362. In the present application, the bulk density of the detergent particles is defined as a bulk density after removing granules exceeding 500 μm by a predetermined sieving process and a pulverization process.

2. Average particle size As for the average particle size, the average particle size depends on the size of the mesh after vibrating for 5 minutes using a metal mesh sieve (mesh opening 2000-45 μm) described in JIS Z8801-1: 2006. The median diameter is calculated from the mass fraction. More specifically, using a 12-stage sieve having a mesh size 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 saucer. 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 (made 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%.

3. Moisture Moisture measurement is performed by infrared moisture meter method. That is, 3 g of a sample is placed on a sample dish having a known mass, heated at 105 ° C. using an infrared moisture meter (FD-240 manufactured by Kett Science Laboratory Co., Ltd.), and drying is completed when the mass change disappears for 30 seconds. And And a moisture content is computed from the mass after drying, and the mass before drying.

4). Flowability The flow time is defined as the time required for 100 mL of powder to flow out from the bulk density measurement hopper defined by JIS K 3362. The flow time is preferably 10 seconds or less, more preferably 8 seconds or less, and even more preferably 7 seconds or less.

  In addition, in this application, the fluidity | liquidity of a detergent particle group shall be the fluidity | liquidity after removing the granule exceeding 500 micrometers by a predetermined sieving process and a grinding | pulverization process.

In the following, aspects of the invention will be further described and disclosed by means of examples. This example is merely illustrative of the invention and is not meant to be limiting in any way. In the following examples and the like, the following raw materials were used unless otherwise specified.
Light ash: average particle size 100 μm (manufactured by Central Glass Co., Ltd .; moisture content 2 mass%)
Zeolite: Average particle size 3.5 μm, manufactured by Zeobuilder

  In the following examples and the like, a 75 L drum granulator (φ40 cm × L60 cm) having a baffle plate was used as the container rotating granulator. As a two-fluid nozzle, manufactured by Atmax Co., Ltd .: model number BN90 was used.

  The invention is further illustrated based on the following examples.

Example 1
Surfactant composition containing an anionic surfactant (R-OSO ₃ Na; C12 / C14 / C16 = 64/24/12 (mass ratio); moisture content 34% by mass; viscosity at 60 ° C .: about 2 Pa · s; hereinafter referred to as “Composition A”) was set to 60 ° C. Next, with respect to 100 parts by mass of Composition A, a mixture comprising 13.2 parts by mass of 2-ethylhexyl glyceryl ether 90% by mass and 10% by mass of water is added and mixed for 1 minute at a temperature of 60 ° C. As a result, “Composition B” was obtained. The viscosity of Composition B at 60 ° C. was 2.4 Pa · s. In composition B, the amount of alkyl glyceryl ether is 18 parts by weight with respect to 100 parts by weight of the anionic surfactant, and the amount of water is 53.52 parts by weight with respect to 100 parts by weight of the anionic surfactant. Met.

  Next, 3.99 kg of light ash was stirred in a drum granulator (rotation speed 30 r / m, fluid number 0.2) having a baffle plate. After stirring for 10 seconds, 75.5 parts by mass of the composition B was added to 100 parts by mass of the light ash using a two-fluid nozzle (Air spray pressure for atomization: 0.3 MPa) at a droplet diameter of about 130 μm. Added in 1 minute. After the addition, the mixture was further granulated by continuing mixing for 1 minute, and then the detergent particles were discharged from the drum granulator. Further, the obtained detergent particles were sieved with a sieve having an opening of 500 μm, and coarse particles of 500 μm or more were pulverized to 500 μm or less with a Fitzmill (manufactured by Hosokawa Micron Co., Ltd., DKA-6 type). It mixed with the granulated material which passed the sieve, and the detergent particle group 1 was obtained.

  The obtained detergent particle group 1 had a water content of 12.6%, an average particle size of 242 μm, a bulk density of 660 g / L, and a fluidity of 7.2 s.

Example 2
To 100 parts by mass of Composition A, 26.4 parts by mass of a mixture of 90% by mass of 2-ethylhexyl glyceryl ether and 10% by mass of water was added and mixed at a temperature of 60 ° C. for 1 minute to obtain a surfactant paste. “Composition C” was obtained. The viscosity of Composition C at 60 ° C. was 2.5 Pa · s. In composition C, the amount of alkyl glyceryl ether is 36 parts by mass with respect to 100 parts by mass of the anionic surfactant, and the amount of water is 55.52 parts by mass with respect to 100 parts by mass of the anionic surfactant. Met.

  Next, 3.8 kg of light ash was stirred in a drum granulator having a baffle plate (rotation speed 30 r / m, fluid number 0.2). After stirring for 10 seconds, 84.2 parts by mass of the composition C was added to 100 parts by mass of the light ash using a two-fluid nozzle (Air spray pressure for atomization: 0.3 MPa) at a droplet diameter of about 130 μm. Added in 3 minutes. After the addition, the mixture was further granulated by continuing mixing for 1 minute, and then the detergent particles were discharged from the drum granulator. Further, the obtained detergent particles were sieved with a sieve having an opening of 500 μm, and coarse particles of 500 μm or more were pulverized to 500 μm or less with a Fitzmill (manufactured by Hosokawa Micron Co., Ltd., DKA-6 type). It mixed with the granulated material which passed the sieve, and the detergent particle group 2 was obtained.

  The obtained detergent particle group 2 had a water content of 12.5%, an average particle size of 248 μm, a bulk density of 706 g / L, and a fluidity of 8.1 s.

Example 3
Surfactant composition containing an anionic surfactant (R—O (CH ₂ CH ₂ O) ₂ SO ₃ Na; C12 / C14 = 70/30 (mass ratio) EO average added mole number 2; moisture 30 mass%; viscosity at 60 ° C .: about 1.9 Pa · s; hereinafter referred to as “composition E”) was set to 60 ° C. Next, with respect to 100 parts by mass of Composition E, 13.2 parts by mass of a mixture of 90% by mass of 2-ethylhexyl glyceryl ether and 10% by mass of water is added and mixed for 1 minute at a temperature of 60 ° C. As a result, “Composition D” was obtained. The viscosity of Composition D at 60 ° C. was 5.9 Pa · s. In composition D, the amount of alkyl glyceryl ether is 18 parts by weight with respect to 100 parts by weight of the anionic surfactant, and the amount of water is 44.88 parts by weight with respect to 100 parts by weight of the anionic surfactant. Met.

  Next, 3.99 kg of light ash was stirred in a drum granulator (rotation speed 30 r / m, fluid number 0.2) having a baffle plate. After stirring for 10 seconds, 61.4 parts by mass of the composition D was added to 100 parts by mass of the light ash using a two-fluid nozzle (Air spray pressure for atomization: 0.3 MPa) at a droplet diameter of about 130 μm. Added in 1 minute. After the addition, the mixture was further granulated by continuing mixing for 1 minute, and then the granulated product was discharged from the drum type granulator. Further, the obtained granulated product was sieved with a sieve having an opening of 500 μm, and coarse particles of 500 μm or more were pulverized to 500 μm or less with a Fitzmill (manufactured by Hosokawa Micron Co., Ltd., pulverizer; DKA-6 type). It was mixed with the granulated material that passed through the sieve, and charged into the drum granulator. Next, 30 parts by mass of zeolite was added to 100 parts by mass of light ash, and the mixture was stirred for 1 minute under the same conditions as described above. The resulting granulated product was discharged from the drum mixer to form detergent particle group 5. .

  The resulting detergent particle group 5 had a water content of 9.7%, an average particle size of 336 μm, a bulk density of 707 g / L, and a fluidity of 6.8 s.

Comparative Example 1
Composition A was brought to 60 ° C. Next, 4.2 kg of light ash was stirred in a drum granulator having a baffle plate (rotation speed 30 r / m, fluid number 0.2). After stirring for 10 seconds, 66.7 parts by mass of the above composition A was added to 100 parts by mass of the light ash using a two-fluid nozzle (Air spray pressure for atomization: 0.3 MPa) at a droplet diameter of about 130 μm. Added in 7 minutes. After the addition, the mixture was further granulated by continuing mixing for 1 minute, and then the detergent particles were discharged from the drum granulator. Further, the obtained detergent particles were sieved with a sieve having an opening of 500 μm, and coarse particles of 500 μm or more were pulverized to 500 μm or less with a Fitzmill (manufactured by Hosokawa Micron Co., Ltd., DKA-6 type). It mixed with the granulated material which passed the sieve, and detergent particle group 3 was obtained.

  The obtained detergent particle group 3 had a water content of 10.7%, an average particle size of 229 μm, a bulk density of 540 g / L, and a fluidity of 6.9 s.

Comparative Example 2
Composition A was brought to 60 ° C. Next, 2.7 kg of light ash was stirred in a Redige mixer (manufactured by Matsubo, capacity 20 L, with jacket). In addition, 40 degreeC warm water was poured into the jacket. After stirring for 10 seconds under conditions of a stirring blade rotation speed of 80 r / m and a shearing machine rotation speed of 3600 r / m, 66.7 parts by mass of the composition A were added to 100 parts by mass of the light ash over 9 minutes. After the addition, the mixture was further granulated by continuing mixing for 1 minute, and then the detergent particles were discharged from the Redige mixer. Further, the obtained detergent particles were sieved with a sieve having an opening of 500 μm, and coarse particles of 500 μm or more were pulverized to 500 μm or less with a Fitzmill (manufactured by Hosokawa Micron Corporation, pulverizer; DKA-6 type). It mixed with the granulated material which passed the sieve, and detergent particle group 4 was obtained.

  The obtained detergent particle group 4 had a water content of 12.8%, an average particle size of 205 μm, a bulk density of 750 g / L, and a fluidity of 7.9 s.

Comparative Example 3
Composition E was brought to 60 ° C. Next, 4.2 kg of light ash was stirred in a drum granulator having a baffle plate (rotation speed 30 r / m, fluid number 0.2). After stirring for 10 seconds, 53.8 parts by mass of the composition E was added to 100 parts by mass of the light ash using a two-fluid nozzle (Air spray pressure for atomization of 0.3 MPa) at a droplet diameter of about 130 μm. Added in 7 minutes. After the addition, the mixture was further granulated by continuing mixing for 1 minute, and then the granulated product was discharged from the drum type granulator. Further, the obtained granulated product was sieved with a sieve having an opening of 500 μm, and coarse particles of 500 μm or more were pulverized to 500 μm or less with a Fitzmill (manufactured by Hosokawa Micron Co., Ltd., pulverizer; DKA-6 type). It was mixed with the granulated material that passed through the sieve, and charged into the drum granulator. Next, 14 parts by mass of zeolite was added to 100 parts by mass of light ash, and the mixture was stirred for 1 minute under the same conditions as described above, and the resulting granulated product was discharged from the drum mixer to form detergent particle group 6. .

  The resulting detergent particle group 6 had a water content of 8.9%, an average particle size of 235 μm, a bulk density of 701 g / L, and a fluidity of 7.1 s.

  Table 1 shows the conditions and results of the above Examples and Comparative Examples.

  In the table, a product of less than 125 μm is a ratio (mass%) occupied by a particle group of less than 125 μm in all detergent particle groups.

  From the comparison between Examples 1 to 3 and Comparative Examples 1 to 3, using a container rotating granulator, a surfactant paste containing an anionic surfactant, alkyl glyceryl ether and water was added with a multi-fluid nozzle. It has been clarified that the solubility of the obtained detergent particles is improved by mixing.

The detergent particle groups of Examples 1 and 2 have a larger average particle size and higher bulk density than the detergent particle group of Comparative Example 1, and therefore, although the decrease in solubility at low temperatures was expected. Surprisingly, it has been found that the low-temperature solubility is improved.
The same applies to the comparison between the detergent particle group of Example 3 and the detergent particle group of Comparative Example 3.

  Furthermore, since the proportion of the detergent particle groups of Examples 1 to 3 less than 125 μm is smaller than Comparative Examples 1 to 3, the production method of the present invention can produce detergent particle groups having a sharp particle size distribution. I understood.

  According to the present invention, using a surfactant paste containing an anionic surfactant, alkyl glyceryl ether and water, detergent particles having a required particle size which is excellent in solubility in low-temperature water and has a sharp particle size distribution. Groups can be produced with good yield. Such a detergent particle group can be used as a constituent component of, for example, a powder detergent for clothing and a detergent for automatic tableware.

Claims (9)

In powder detergent raw materials, the following a) component, c) component and b) component:
a) Anionic surfactant
c) Alkyl glyceryl ether
b) A method for producing a detergent particle group including a surfactant paste mixing step in which a surfactant paste containing water is added using a multi-fluid nozzle and mixed by a container rotating granulator. a) An anionic surfactant is represented by the following formula (1):
R—O—SO ₃ M (1)
(In the formula, R represents an alkyl group or alkenyl group having 10 to 18 carbon atoms, and M represents an alkali metal atom, ammonia or an amine.)
The manufacturing method of Claim 1 which is a compound represented by these.   The manufacturing method of Claim 1 or 2 which uses 10-40 mass parts of c) alkyl glyceryl ether with respect to 100 mass parts of a) anionic surfactant.   The manufacturing method of any one of Claims 1-3 whose quantity of b) water in surfactant paste is 25-70 mass parts with respect to 100 mass parts of a) anionic surfactant.   The production method according to any one of claims 1 to 4, wherein the powder detergent raw material is a powder detergent raw material containing light ash and / or sodium sulfate.   The manufacturing method of any one of Claims 1-5 which adds 25-200 mass parts surfactant paste with respect to 100 mass parts of powder detergent raw materials.   The manufacturing method of any one of Claims 1-6 whose average particle diameter of a detergent particle group is 150-800 micrometers.   The detergent particle group obtained by the manufacturing method of any one of Claims 1-7.   The detergent composition formed by containing the detergent particle group obtained by the manufacturing method of any one of Claims 1-7.