JPH11140498A - Method for producing high bulk density granular detergent composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for producing a high bulk density granular detergent composition in which a liquid acid precursor of an anionic surfactant is dry-neutralized and granulated with a solid alkali inorganic material, and is suitable for reducing coarse particles and fine powder. Provided is a production method capable of obtaining a product having a high particle density and a high particle size. SOLUTION: A mixer / granulator is used to stir and mix an acid precursor solution of an anionic surfactant and a powder containing a particulate alkali inorganic material having a neutralization equivalent or more, and neutralize and granulate the obtained powder. The granulated material is crushed by a crusher equipped with a rotary blade,
And a crushing and granulating step of crushing under the conditions described above.
Tip speed (peripheral speed) of rotary blade: 10 to 60 m / s, screen hole diameter: 1.2 mm or more Processing capacity: 5 to 30 t / m
² hr (per area of screen opening per hour)

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a method for producing a high bulk density granular detergent composition, and more particularly to a method for producing a high bulk density granular detergent composition including neutralization of an acid precursor of an anionic surfactant.

[0002]

2. Description of the Related Art In the detergent industry, attention has recently been paid to a method for producing a detergent without using a spray drying method which requires a large amount of energy and space. A production method including neutralizing an acid precursor of an anionic surfactant with a solid alkali inorganic material is one of the particularly important ones. That is, a method for producing a high bulk density detergent using an acid precursor of an anionic surfactant (water content of 1% or less) as a starting material requires a neutralization step, but the surfactant which is the mainstream of the current detergent production method is used. Unlike the production method using an aqueous slurry (water content of 30 to 70%) as a starting material, a large-scale spray-drying device is not required, so that there are advantages of low equipment cost and energy saving.

A method for producing a granular detergent using an acid precursor of an anionic surfactant as a starting material is disclosed in JP-A-60-72.
998, JP-A-60-72999, JP-A-61-6
No. 6798 proposes a method in which an unneutralized sulfonate is neutralized and mixed with sodium carbonate and water by a strong shearing device, cooled, aged, and further pulverized and granulated. However, these methods have drawbacks in that a large power is required due to the use of a powerful shearing device, and that the neutralized product is bulky, so that a cooling / aging process and a pulverizing process must be provided in the next step.

[0004] In order to solve these problems, several methods have been proposed for neutralizing and granulating in a high-speed mixer / granulator having both a stirring function and a shearing function. For example, JP-A-3-33199 discloses that an acid precursor of an anionic surfactant is added to a solid inorganic alkali substance fluidized in a high-speed mixer / granulator while maintaining the temperature at 55 ° C. or lower, Methods for performing neutralization and granulation have been proposed.
However, this method has the disadvantage that the temperature must be kept below 55 ° C. and a long neutralization time is required.

Further, JP-A-4-363398 discloses that an acid precursor of an anionic surfactant is gradually added to a solid alkali-inorganic material in a high-speed mixing / granulating machine, and the mixture is kept in a particulate state. A batch method in which the mixture is neutralized and then granulated in the presence of a liquid binder.
No. 00 regulates the water content of the product to 5 to 15%,
A single-step continuous production method has been proposed in which neutralization of the anionic surfactant acid precursor with the solid alkaline inorganic material is achieved in a high-speed mixer / granulator at 80% or more. However, the former method is not suitable for mass production because it is a batch process, it is difficult to suppress the formation of large lumps during the neutralization reaction, and the neutralization reaction time must be relatively long. There is a drawback, and in order to solve the formation of large lumps, it is conceivable to carry out a crushing treatment after granulation, but the crushing treatment causes a problem of generation of fine powder. In the latter method, in order to shorten the residence time in the apparatus (5 to 30 seconds), the water content of the treated material for promoting the neutralization reaction is strictly limited to 5 to 15%. For example, liquid components that can be exceeded, for example, cannot be blended directly, or the neutralized material moisture is determined by the moisture brought in from the raw material to be treated. It has the drawback that the water content is high, that is, there is not much freedom in the water balance, and further, depending on the conditions, a complete neutralization reaction cannot be achieved.

[0006]

SUMMARY OF THE INVENTION Accordingly, an object of the present invention is not to use a spray drying method, but to mix and granulate an acid precursor of an anionic surfactant and a granular alkali inorganic material by a stirring granulation method to obtain a granular detergent. In the so-called stirring granulation non-tower process for producing the composition, the generation of fine powder and coarse particles is suppressed,
It is an object of the present invention to provide a method for producing a high bulk density granular detergent composition having a suitable particle size.

[0007]

Means for Solving the Problems The inventors of the present invention have conducted intensive studies to achieve the above object, and as a result, the acid precursor of the anionic surfactant and the granular alkaline inorganic material were mixed in a mixer / granulator. The resulting powder is stirred and mixed, neutralized, and granulated, and then the granulated material is crushed under specific conditions to obtain a high bulk density granular detergent composition having an appropriate particle size with suppressed generation of fine powder. And found that the present invention was completed.

That is, according to the present invention, there is provided a method for producing a high bulk density granular detergent composition comprising a neutralization reaction of an acid precursor of an anionic surfactant with a granular alkaline inorganic material and a granulation step. In a mixer / granulator equipped with a function and a shearing function, the powder containing the acid precursor of the anionic surfactant and the granular alkali inorganic material having a neutralization equivalent or more is neutralized,
Neutralization, granulation process, which performs granulation to prepare granules, and b)
The above granulated product is crushed by a pulverizer equipped with a rotary blade.
Crushing and granulating step of crushing under the following conditions: Tip speed (peripheral speed) of rotary blade: 10 to 60 m / s, Screen hole diameter: 1.2 mm or more Processing capacity: 5 to 30 t / m ² · hr (Screen opening area (Per hour) and a method for producing a high bulk density detergent composition.

[0009]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail. The method for producing a high bulk density granular detergent composition of the present invention comprises a neutralization reaction between an acid precursor of an anionic surfactant and a granular alkali inorganic material and a granulation step, and has a stirring function and a shearing function. Preparing a granulated product by stirring and mixing a powder containing an acid precursor of an anionic surfactant and a granular alkali inorganic material having a neutralization equivalent or more with a mixer / granulator, neutralizing and granulating. And a step of crushing the granulated material by a crusher equipped with a rotary blade under the following conditions. Tip speed (peripheral speed) of rotary blade: 10 to 60 m / s, screen hole diameter: 1.2 mm or more Processing capacity: 5 to 30 t / m ² · hr (per screen opening area / time)

Surfactants and / or directly without spray drying
Alternatively, in a method of producing a granular detergent composition by mixing and granulating a precursor thereof and an alkali inorganic material by a stirring granulation method, coarse particles are often generated when an attempt is made to obtain a granular material having a high bulk density. Therefore, when the generated coarse particles are crushed under ordinary conditions, fine powder is generated. In the present invention, by performing pulverization under the above-described specific conditions, pulverization can be performed while maintaining a high bulk density and without increasing fine powder.

In the present invention, first, a mixer / granulator having a stirring function and a shearing function is used to stir and mix a powder containing an acid precursor of an anionic surfactant and a particulate alkali inorganic material having a neutralization equivalent or more. , Neutralization and granulation are performed to prepare a granulated product.

In the method of the present invention, the acid precursor of the anionic surfactant includes a known anionic surfactant such as linear alkylbenzenesulfonic acid, α-olefinsulfonic acid, alkyl sulfate, polyoxyethylene alkyl ether sulfate, etc. The acid precursor of the activator is arbitrarily selected from alone or in combination. In addition, as the granular alkali inorganic material, any material can be used, and preferably, sodium carbonate and potassium carbonate, or an alkali builder combining them. Upon neutralization of the acid precursor solution of the anionic surfactant and the granular alkali builder, a neutral alkali equivalent or more of the solid alkali builder is added to the acid precursor solution.

In the neutralization reaction, apart from the acid precursor of the anionic surfactant and the granular alkali inorganic material, other components commonly found in detergents may be supplied in any amount and in any combination. it can. In this case, examples of other components that can be supplied include an aqueous solution of an anionic surfactant metal salt such as an α-olefin sulfonate metal salt and an α-sulfo fatty acid ester metal salt, a nonionic surfactant, soap, zeolite, and tripolyphosphate. Materials generally known as detergent components such as soda, an anti-redeposition agent (such as carboxymethyl cellulose), a fluorescent agent, and an extender (such as sodium sulfate) can be used. These materials can be arbitrarily and directly supplied to the apparatus in one kind or a combination of two or more kinds.

The neutralization / granulation step of the present invention is carried out in a mixer / granulator having a stirring function and a shearing function. By using the mixer / granulator, a good fluidized state of the granular alkaline inorganic material can be formed before the introduction of the acid precursor liquid of the anionic surfactant, thereby maintaining the reaction mixture in a granular form. Easier to do.

[0015] The mixer / granulator preferably comprises a rotary stirrer and a shearing member operable independently of each other at independently variable speeds. For example, Ledige Mixer [Matsubo Co., Ltd.], High Speed Mixer [Fukae Kogyo Co., Ltd.], Grall [Fuji Paudal Co., Ltd.]
And Spiraflow [manufactured by Freund Corporation].

In performing this step, it is preferable to perform jacket cooling because heat is generated by neutralization. Further, it is preferable to carry out the operation at a volume ratio of 10 to 60%, and it is preferable to carry out the operation while rotating the chopper (sub shaft) at high speed in order to suppress generation of coarse powder.

In the present invention, the granulated product obtained in the neutralization / granulation step is then sent to the crush granulation step. In this step, the granulated material is crushed with a rotary blade,
It is crushed under the following conditions. Tip speed (peripheral speed) of rotary blade: 10 to 60 m / s, screen hole diameter: 1.2 mm or more Processing capacity: 5 to 30 t / m ² · hr (per screen opening area / time)

This step is carried out by using an impact, cutting or shearing type pulverizer under the above conditions. When the tip speed of the rotary blade exceeds 60 m / s, generation of fine powder is remarkable, and when it is less than 10 m / s, the amount of coarse powder does not decrease. When the screen hole diameter is less than 1.2 mm, the generation of fine powder is remarkable. If the processing capacity is less than 5 t / m ² · hr, the amount of generated fine powder is large, and if the processing capacity is more than 30 t / m ² · hr, a short path is generated, and the coarse powder content is increased.

In the present step, it is preferable to maintain the temperature at less than 45 ° C.
The following is preferred. Further, in this step, the addition of a grinding aid is effective in improving the powder properties, and is therefore preferable. In this case, examples of the grinding aid include powders such as zeolite, sodium carbonate, potassium carbonate, and titanium oxide, and those having an average particle diameter of 20 μm or less are preferable. The addition amount is suitably not more than 10% by weight of the whole produced powder, more preferably 2 to 6% by weight. In addition,
Other components of the above-described detergent can also be added in this step.

As the pulverizer, any type of impact, cutting or shearing type can be used. For example, a speed mill (manufactured by Okada Seiko Co., Ltd.), Fitzmill (manufactured by Hosokawa Micron Corporation), Komi Nuter [Fuji Paudal Co., Ltd.], Pulverizer [Tokyo Atomizer Co., Ltd.]
Manufactured).

According to this step, a crushed granule having a bulk density of 0.6 g / cc or more, preferably 0.7 g / cc or more is formed. The average particle size of the final crushed granules is 200-700μ
m is appropriate and preferably 300 to 500 μm. Those having a particle size of 1000 μm or more are 20% or less, preferably 10% or less, and those having a particle size of 150 μm or less are 20% or less, preferably 10% or less.

The following is a summary of the embodiments of the present invention. (1) A method for producing a high bulk density granular detergent composition including a neutralization reaction between an acid precursor of an anionic surfactant and a granular alkaline inorganic material and a granulation step, i) a mixer having a stirring function and a shearing function / With a granulator,
A neutralization and granulation step in which a powder containing an acid precursor of an anionic surfactant and a granular alkali inorganic material having a neutralization equivalent or more is stirred and mixed, and neutralization and granulation are performed to prepare a granulated product; ) A crushing and granulating step of crushing the above-mentioned granulated material by a crusher equipped with a rotary blade under the following conditions: a tip speed (peripheral speed) of the rotary blade: 10 to 60 m / s; a screen hole diameter: 1.2 mm A method for producing a high bulk density detergent composition comprising: a treatment capacity of 5 to 30 t / m ² · hr (perforated area of screen / per hour). (2) The method according to the above (1), wherein cold air is introduced in the crushing and granulating step. (3) The method according to the above (1), wherein a grinding aid is added in the crushing and granulating step.

[0023]

The present invention will be described in more detail with reference to the following Examples, which should not be construed as limiting the technical scope of the present invention.

Examples 1 to 7 and Comparative Examples 1 and 2 Granular solid alkali (sodium carbonate) and powdered alkali builder (sodium tripolyphosphate, zeolite) and other (CBS) were granulated in a ratio shown in Table 1 by a granulator [Lady Gemixer, FKM-50D, manufactured by Matsubo Co., Ltd.], the main shaft was operated at a rotation speed of 150 rpm for 1 minute, and then the liquid acid precursor (LAS-H) was charged in a stationary state. Perform neutralization granulation under the conditions. After completion of the neutralization granulation, a coating agent (zeolite) was added at the ratio shown in Table 1 and then fluidized under the conditions shown in Table 2 for 3 minutes, discharged from the granulator and neutralized as shown in Table 2. Granules were obtained. Next, this neutralized granulated product was pulverized with a pulverizer [Fitz Mill DK].
AS06, manufactured by Hosokawa Micron Co., Ltd.] under the grinding conditions shown in Table 3 to obtain a ground product. Table 3 shows the properties of the obtained pulverized product.

[0025]

[Table 1]

[0026]

[Table 2]

[0027]

[Table 3]

[0028]

According to the present invention, there is provided a method for producing a high bulk density detergent composition by stirring granulation of an acid precursor of an anionic surfactant and a granular alkali inorganic material. An acid precursor solution of the activator and a powder containing a granular alkali inorganic material having a neutralization equivalent or more are stirred and mixed, neutralized, neutralized to prepare a granulated product by performing granulation, and a granulation step,
Since the above-mentioned granulated product includes the crushing and granulating step of crushing under the above-mentioned specific conditions by a crusher having a rotary blade, the following outstanding effects are exhibited. A) A product having a high bulk density can be obtained. B) It can be manufactured with a simple device. C) A product with less coarse and fine powder can be obtained.

Continued on the front page (72) Inventor Isao Nishimura 1-3-7 Honjo, Sumida-ku, Tokyo Inside Lion Corporation

Claims (1)

[Claims] 1. A method for producing a high bulk density granular detergent composition comprising a neutralization reaction between an acid precursor of an anionic surfactant and a granular alkali-inorganic material and a granulation step, i) having a stirring function and a shearing function With a mixer / granulator
A neutralization and granulation step in which a powder containing an acid precursor of an anionic surfactant and a granular alkali inorganic material having a neutralization equivalent or more is stirred and mixed, and neutralization and granulation are performed to prepare a granulated product; ) A crushing and granulating step of crushing the above-mentioned granulated material by a crusher equipped with a rotary blade under the following conditions: a tip speed (peripheral speed) of the rotary blade: 10 to 60 m / s; a screen hole diameter: 1.2 mm A process for producing a detergent composition having a high bulk density, comprising: a treatment capacity of 5 to 30 t / m ² · hr (perforated area of screen / per hour).