JPH07268396A - Production of granular nonionic detergent composition - Google Patents

Abstract

PURPOSE:To provide a method for producing the subject composition, capable of readily controlling granulating time, particle diameter and bulk density. CONSTITUTION:In producing a granular nonionic detergent composition by stirring and granulating (a) 10-70wt.% of a nonionic surfactant, (b) 5-50wt.% of crystalline aluminosilicate, (c) >=0.2wt.% and <5wt.% of porous inorganic oxide powder and (d) 1-75wt.% of sodium carbonate, 1-90wt.% of at least either one component of these components (b), (c) and (d) used for granulation is left as powder for additionally adding and stirring, and granulation is started and the powder for additionally adding is added thereto within a period from the start of addition to the completion of stirring and granulating treatment.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a granular detergent composition containing a nonionic surfactant as a main component, which is easy to control granulation. The present invention also relates to a method for producing a granular detergent composition containing a nonionic surfactant as a main component, which has improved dust generation.

[0002]

2. Description of the Related Art Nonionic surfactants generally have a low foaming property, their detergency is hardly affected by the hardness of water, and they are particularly excellent in dirt dispersibility and stain dispersibility at low temperatures. Furthermore, it is an excellent surfactant with good biodegradability, low environmental load, low toxicity and no safety problem. Examples of the method for producing a granular detergent containing a nonionic surfactant as a main component include, for example, JP-A-52-101121 and JP-A-62-2632.
Various methods have been proposed in Japanese Patent Laid-Open No. 99, Japanese Patent Laid-Open No. 57-159898, and the like.

However, nonionic surfactants are generally liquid at room temperature, and there is a problem that granulation control is not easy in production by stirring granulation. So far, this issue has not been sufficiently studied. Further, as described above, since the nonionic surfactant is generally liquid at room temperature, there is a concern that the nonionic surfactant exudes from the nonionic granular detergent product into the detergent container. Therefore, Japanese Patent Laid-Open No. 4-
In 339898, an amorphous oil-absorbing carrier is used in an amount of 5-2.
It has been proposed to improve the exudation of the nonionic surfactant by adding 0%.

Although it is possible to improve "bleeding" by adding the above oil-absorbing carrier, when a large amount of such a non-washing component is mixed in a detergent, it is a powder at the time of use during washing. However, there is a problem in that workability is deteriorated and discomfort is caused by "sucking".

[0005]

DISCLOSURE OF THE INVENTION An object of the present invention is to produce a granular nonionic detergent composition by stirring granulation with easy granulation control. The present invention also aims to produce a granular nonionic detergent composition with improved dusting properties.

[0006]

[Means for Solving the Problems] As a result of intensive studies on the above problems, at least one component of a crystalline aluminosilicate, a porous inorganic oxide powder and sodium carbonate used as a powder raw material in stirring granulation is found. At the start of agitation granulation, a part of the above is reserved for additional addition without being added to the agitation granulator, and the rest is used with other powder raw materials and nonionic surfactant to start agitation granulation. After that, by adding the crystalline aluminosilicate porous inorganic oxide powder or sodium carbonate for additional addition described above and continuing and completing the stirring granulation, it was found that the granulation control becomes easy. Completed the invention.

Further, a part or all of the porous inorganic oxide powder in the detergent raw material is preliminarily dispersed in a nonionic surfactant, and further aluminosilicate, the remaining porous inorganic oxide powder, and sodium carbonate. By stirring and granulating with
The present invention has been completed by finding that the above dust generation problem can be solved.

That is, in the first method for producing a granular nonionic detergent composition of the present invention (hereinafter referred to as method A), the following components (a) to (d) are used in the following amounts, respectively, and stirred granulation is carried out. In producing the granular nonionic detergent composition, (a) nonionic surfactant: 10 to 70% by weight (b) crystalline aluminosilicate: 5 to 50% by weight (c) porous inorganic oxide powder: 0.2% by weight or more and less than 5% by weight (d) Sodium carbonate: 1 to 75% by weight of the amount of at least one of the above-mentioned components (b), (c) and (d) used for granulation 1 to 90 out of
% (Weight basis) is left as a powder for additional addition, and the remaining components (b), (c), (d) and (a) are added to the stirring granulator to start stirring granulation. However, the powder for additional addition is added all at once or in a divided or continuous manner until the end of the stirring granulation treatment, and the stirring granulation is continued to form detergent particles.

A second method for producing a granular nonionic detergent composition of the present invention (hereinafter referred to as method B) is as follows (a).
(A) Nonionic surfactant: 10-70% by weight (b) Crystalline aluminosilicate: 5 to 50 wt% (c) Porous inorganic oxide powder: 0.2 wt% or more and less than 5 wt% (d) Sodium carbonate: 1 to 75 wt% Preliminary porous inorganic oxide of component (c) 5% of powder
The nonionic surfactant of the component (a) is dispersed on the above (weight basis), the obtained dispersion, (b) the crystalline aluminosilicate, the rest (c) the porous inorganic oxide powder and (d). It is characterized in that sodium carbonate is granulated with stirring to form detergent particles.

[0010]

BEST MODE FOR CARRYING OUT THE INVENTION Examples of the nonionic surfactant as the component (a) used in the present invention include the following. (1) C3-C22, preferably C8-C18 aliphatic alcohol with C2-C4 alkylene oxide on average 3
-30 mol, preferably 7-20 mol added polyoxyalkylene alkyl (or alkenyl) ether.
Among these, polyoxyethylene alkyl (or alkenyl) ether and polyoxyethylene polyoxypropylene alkyl (or alkenyl) ether are preferable.

(2) Polyoxyethylene alkyl (or alkenyl) phenyl ether (3) General formula (I) of the following chemical formula 1 in which alkylene oxide is added between ester bonds of long-chain fatty acid alkyl ester.
Fatty acid alkyl ester alkoxylate

[0012]

Embedded image R ₁ CO (OA) nOR ₂ (I) (R ₁ CO: C 6-22, preferably 8-18 fatty acid residue OA: 2-4 carbon atoms such as OCH ₂ CH ₂ ; Preferably 2
Addition unit of alkylene oxide of 3 n: Shows the average number of moles of addition of alkylene oxide, 3 to
30, preferably a number of 7 to 20 R ₂ : a lower alkyl group having 1 to 3 carbon atoms) (4) Polyoxyethylene sorbitan fatty acid ester (5) Polyoxyethylene sorbit fatty acid ester (6) Polyoxyethylene fatty acid ester (7 ) Polyoxyethylene hydrogenated castor oil (8) Glycerin fatty acid ester

Among the above nonionic surfactants, polyoxyethylene alkyl (or alkenyl) ethers,
A fatty acid methyl ester ethoxylate obtained by adding ethylene oxide to a fatty acid methyl ester is particularly preferably used.

The nonionic surfactant as the component (a) is 10
˜70% by weight, preferably 10 to 60% by weight, and the mixture is agitated and granulated. If this amount is less than 10% by weight, the excellent cleaning properties of the nonionic surfactant cannot be utilized, while if it exceeds 70% by weight, the adhesion to the inside of the agitation granulator is significantly increased and granulation becomes difficult. Become.

As the crystalline aluminosilicate as the component (b), synthetic zeolite having an average particle size of 0.1 to 10 μm is preferably used. The crystalline aluminosilicate as the component (b) is blended in an amount of 5 to 50% by weight, preferably 20 to 40% by weight and stirred and granulated. If the blending amount is less than 5% by weight, the granulated product becomes lumpy or becomes pasty and cannot be granulated. On the other hand, if it exceeds 50% by weight, the granulating time is prolonged and the production capacity is lowered.

As the porous inorganic oxide powder as the component (c), one having a SiO ₂ content of 50% by weight or more is suitable, and amorphous silica (trade name: TOKUSIL (Tokuyama Soda),
Aerosil (Japan Aerosil), crystalline calcium silicate (trade name: Florite (Tokuyama Soda)), crystalline magnesium silicate (trade name: Wollastonite (Hayashi Kasei))
And so on.

The porous inorganic oxide powder of the component (c) is
It is blended in an amount of 0.2% by weight or more and less than 5% by weight, preferably 1 to 4% by weight and mixed by stirring. This blending amount is 0.
If it is less than 2% by weight, the granulated product becomes lumpy or paste-like and cannot be granulated. On the other hand, if it is 5% by weight or more, the dust generation property of the product is deteriorated and problems such as "sem" occur during use.

As the sodium carbonate as the component (d), heavy sodium carbonate having a high bulk density (trade name: granular ash (Asahi Kasei)), light sodium carbonate having a low bulk density (trade name: light ash (Asahi Kasei)), etc. There is. The component (d), sodium carbonate, is blended so as to be contained in an amount of 1 to 75% by weight and granulated with stirring. When the blending amount is 75% by weight or more, the granulation time becomes long and the production is lowered. Further, it is preferable to add 10% by weight or more of sodium carbonate as the component (d), which improves the fluidity of the product.
The component (d) sodium carbonate is preferably 10 to 60.
It is compounded in an amount of% by weight.

In the granular nonionic detergent composition of the present invention,
The following components which are usually blended in detergent raw materials can be blended, and these may be blended in a solid detergent at the time of stirring and mixing, or may be powder-mixed with the detergent particles obtained by granulation. Good.

(1) Inorganic alkali builder: potassium carbonate, sodium sulfite, sodium silicate, etc. (2) Fluorescent agent: bis (triazinylamino) stilbenedisulfonic acid derivative, bis (sulfostyryl) biphenyl salt [Tinopearl CBS], etc. (3) Enzyme: lipase, protease, cellulase, amylase, etc. (4) Bleach: Percarbonate such as sodium percarbonate, perborate, etc. (5) Antistatic agent: dialkyl type quaternary ammonium salt,
Tertiary amines, etc. (6) Surface modifiers: bentonite, kaolinite, etc.

Next, regarding a specific stirring granulation step,
Method B and method B will be described in this order. In the method A of the present invention, at least the crystalline aluminosilicate of the component (b), the porous inorganic oxide powder of the component (c) and the sodium carbonate of the component (d) which are added at the time of stirring granulation are used. A part of one component is left as a powder for additional addition, and the rest (initial addition amount) is put into a stirring granulator together with other powder raw materials to start stirring, and a nonionic surfactant of the component (a) is added. Is added to the inside of the apparatus by spraying or the like to start stirring granulation. After the start of the stirring granulation and before the end of the stirring granulation, the remaining powder for additional addition is added and the stirring granulation is continued to obtain an average particle size of 3
Detergent particles of 00-3000 μm are obtained. After completion of the stirring granulation, a fluidity improving agent such as zeolite fine powder is added, and if necessary, powder components are mixed with powder, and a fragrance is sprayed to obtain the product of the present invention.

The initial added amount is used for granulation (b),
It is at least one of the components (c) and (d), and is 10 to 99% (weight basis), preferably 20 to 80% of the amount of the component used. in this way,
A part of components (b), (c) and (d) is always added initially. If the amount of each of the components (b), (c), and (d) initially added is less than 10%, the granulated product is lumped and granulation becomes impossible.

On the other hand, at the time of additional addition, (b),
At least one of the components (c) and (d) is additionally added. This addition amount is used in the stirring granulation (b),
1 to 90 of each of the components (c) and (d)
% (Weight basis) is suitable, preferably 3 to 80%. If the amount of this additional addition is less than 1%, the effect of improving the granulation property is weak, while if it is more than 90%, the granulated product is lumped and granulation becomes impossible.

FIG. 1 shows a flow sheet of the above process.
The above-mentioned additional addition may be carried out by adding the remaining total amount in a lump, adding it in two or more divided portions, or adding the total amount of the additional component in small amounts continuously.

Since at least one of the above-mentioned components (b), (c), and (d) may be additionally added, the other components may be initially added in a total amount. in this way,
By adding at least one of the components (b), (c) and (d) in divided portions, granulation control becomes easy and a granular nonionic detergent composition can be easily produced by stirring granulation.

On the other hand, in the method B of the present invention, prior to stirring granulation, a part or all of the porous inorganic oxide of the component (c) is dispersed in the nonionic surfactant of the component (a). The amount of dispersion is at least 15% (weight basis) in the porous inorganic oxide powder of component (c), preferably 10% or more.

Then, the obtained dispersion and the other essential components, that is, the crystalline aluminosilicate as the component (b), the remaining porous inorganic oxide powder as the component (c) and sodium carbonate as the component (d) or Further, other optional components are stirred and granulated to obtain powdery or granular detergent particles having an average particle size of 300 to 3000 μm.

In any of the above methods A and B,
A fluidity improver may be added to the detergent particles obtained by stirring and granulation to improve the fluidity characteristics. As a fluidity improver, the amount passed by JIS200 mesh sieve is 50
%, An inorganic powder is preferable, and examples of the material include carbonates such as sodium carbonate and calcium carbonate, amorphous silica, silicates such as calcium silicate and magnesium silicate, and aluminos such as zeolite. A silicate or the like is used.

The flow improver is added to the composition of the present invention in an amount of 0.
The amount used is preferably 5 to 15% by weight, more preferably 1 to 10% by weight. Furthermore, if desired, other optional components such as an enzyme can be externally added by powder mixing.

[0030]

According to the method A of the present invention, (b) crystalline aluminosilicate and / or (c) porous inorganic oxide powder are dividedly charged and agitated and granulated to control granulation. A granular nonionic detergent composition can be easily manufactured.
Specific examples of the granulation control here include control of the granulation time, the particle size, and the bulk density.

Further, according to the method B of the present invention, a part or all of the previously prepared porous inorganic oxide powder is dispersed in the nonionic surfactant, and then this dispersion, the crystalline aluminosilicate, and the residual substance are dispersed. By stirring and granulating the porous inorganic oxide powder and the sodium carbonate described above, a granular nonionic detergent composition with improved dust generation during production and from the product can be obtained.

[0032]

EXAMPLES In the examples, each sample was evaluated by the following test methods. [Evaluation of Granulation] A sample in the middle of granulation was observed, and if the time required for granulation was too short, granulation control was difficult, and if it was too long, the production capacity was poor. ◯: Time to reach average particle size of 400 μm is 1 minute to 2
0 minutes ×: The time to reach the average particle size of 400 μm is less than 1 minute or more than 20 minutes, or the whole is pasty or violently lumped immediately after the addition of the nonionic surfactant to make granulation impossible.

[Evaluation Method of Dust Generation during Manufacturing] When discharging the product, the discharge port of the Reedige mixer (Matsuzaka Giken Co., Ltd., 20 liter capacity) was observed, and the dust generation state was visually observed according to the following criteria. evaluated. ○: No dust is generated △: A little dust is observed ×: A lot of dust is observed

[Evaluation method of dust generation during use] Using an actual washing machine, drop a spoonful (about 25 g) of detergent from a height of about 70 cm in an empty washing tub to check the dust generation state. It was visually evaluated according to the following criteria. ○: No dust is generated △: A little dust is observed ×: A lot of dust is observed

Examples 1 to 6 The initial additions of the powder raw materials shown in Table 1 (total amount of 8 liters), that is, fine zeolite, amorphous silica and sodium carbonate were added to a Loedige mixer (Matsusaka Giken Co., Ltd.).
Manufactured by M20 type, and the stirring of the main shaft (200 rpm) and the chopper (6000 rpm) was started. The amount of nonionic surfactant shown in Table 1 was added thereto for 1 minute, and the mixture was stirred and granulated. During stirring, samples are taken over time to measure the average particle size, and when the average particle size reaches 300 μm, the remaining powder raw material (additional addition amount) that has been divided is added and stirring granulation is continued. A granulated product was obtained.

Here, in Examples 1 to 5, the additional addition component was added all at once, and in Example 6, it was added continuously. After granulation, 5% of fine particle zeolite is used as a fluidity improver.
The product was added. The granulation property and bulk density were evaluated, and the results are shown in Table 1.

Comparative Examples 1 to 2 Using the raw materials shown in Table 1, stirring granulation was carried out in the same manner as in Examples to evaluate the granulation property.

[0038]

[Table 1]Table 1: Detergent composition and evaluation results Example Comparative example 1 2 3 4 5 6 1 2 Composition (% by weight): Initial addition (a) Nonionic surfactant AE nonion 25 25 25 − − − 25 − FME nonion − − − 25 25 25 − 25 (b) Fine zeolite 15 18 22 25 25 20 5 − ( c) Porous inorganic oxide powder 4 4 4 2 4 2 4 4(d) Sodium carbonate 33 33 33 33 20 20 33 33 Additional additive (b) Fine zeolite 10 7 3 − − 5 20 25 (c) Porous inorganic oxide powder − − − 2 − 2 − −(d) Sodium carbonate − − − − 13 13 − − Water / impurity balance Evaluation results: Granulation ○ ○ ○ ○ ○ ○ × × Bulk density (g / cm ³ ) 0.8 0.9 1.0 1.0 0.8 0.7 − − * 1: Continuous addition (Note) AE nonion: Saturated alcohol with 12 to 15 carbon atoms
Ethylene oxide on average 9 mol adduct (Lion Chemical
(Manufactured by Dovanox 25I) FME Nonion: C₁₁H_{twenty three}CO (OCH₂CH₂)₉OC
H₃(Lion Chemical Co., Ltd., fatty acid methyl ethoxylate
Fine zeolite: Shilton B (manufactured by Mizusawa Chemical Co., Ltd.) Porous inorganic oxide powder: Amorphous silica (Tokushiru N,
Tokuyama Soda Co., Ltd. Sodium carbonate: Asahi Glass Co., Ltd., light ash

The granular nonionic detergent compositions having the compositions obtained in Examples 1 to 6 were further powder-mixed with 0.1% by weight of an enzyme and 0.2% by weight of a fragrance was sprayed to perform actual washing. However, it was confirmed that there were no particular problems and that both quality and performance were good.

Examples 7, 9 and 10 A powder raw material (total volume of 8 liters) obtained by removing the porous inorganic oxide powder from the composition shown in Table 2 was used as a Ledige mixer (M20 manufactured by Matsuzaka Giken Co., Ltd.). Into the main shaft (200r)
pm) and chopper (6000 rpm) stirring was started. Then, the whole amount of the nonionic surfactant having the composition shown in Table 1 in which the porous inorganic oxide was dispersed was added in 1 minute, and the mixture was stirred and granulated. Agitation granulation was performed until the average particle size reached 400 μm, and 5% of fine particle zeolite was added as a fluidity improver to obtain a product. The dust generation property at the time of manufacturing and use of the product was evaluated, and the results are shown in Table 2.

Example 8 0.4% by weight of porous inorganic oxide powder in the composition shown in Table 2
And other powder raw materials (total volume of 8 liters) were put into a Ledige mixer (M-20 type, Matsuzaka Giken Co., Ltd.), and the spindle (20
(0 rpm) and chopper (6000 rpm) were started, and the total amount of the nonionic activator having the composition shown in Table 2 and the remaining porous inorganic oxide powder (3.6% by weight) dispersed therein was reduced to 1 minute. Add and stir granulate. Hereinafter, Example 4
A product was obtained in the same manner as above, and the evaluation results are shown in Table 2.

Comparative Examples 3 and 4 Powder raw materials (total volume: 8 liters) having the compositions shown in Table 2 were put into a Ledige mixer (M-20 type, Matsuzaka Giken Co., Ltd.), and a spindle (200 rpm) and a chopper (6000 rp).
The stirring of m) was started. Then, the entire amount of the nonionic surfactant having the composition shown in Table 2 was added in 1 minute. Average particle size 400μm
Granulation was performed until 5% of fine particle zeolite was added as a fluidity improver to obtain a product. The dusting properties were evaluated at the time of production and at the time of using the product, and the results are shown in Table 2.

Comparative Examples 5 and 6 The compositions shown in Table 1 were evaluated in the same manner as in the Examples. The results are shown in Table 2. The above results are shown in Table 2 below.
Shown in.

[0044]

[Table 2]Table 2: Detergent composition and evaluation results Example Comparative example 7 8 9 10 3 4 5 6 Composition (% by weight): (a) Nonionic surfactant AE nonion 20-25-30-30-25-FME nonion-25-25-40-25-25 (b) Fine zeolite 10 25 25 41 2 25 25 25 (c) Porous Inorganic oxide powder to nonion addition amount * 1 4 0.4 4 4 − − 15 10 to powder raw material addition amount * 2 −3.6 − − 15 15 2 − (d) Sodium carbonate 39 33 33 − 40 22 20 27 Water and impurity balance Evaluation results: Dust generation during manufacturing ○ ○ ○ ○ × × * 3 * 3 Dust generation during use ○ ○ ○ ○ × × * 3 * 3 (Note) * 1) Porous non-dispersed nonionic surfactant
Oxide powder * 2) Porous inorganic oxide added with other powder materials
Powder * 3) Porous inorganic oxide powder for nonionic surfactant
Gelation occurs at the time of addition and cannot be added. AE nonion: A saturated alcohol having 12 to 15 carbon atoms.
Tylene oxide average 9 mole adduct (Lion Chemical Co., Ltd.)
Manufactured by Dovanox 25I) FME Nonion: C₁₅H₃₁CO (OCH₂CH₂)₈OC
H₃(Lion Chemical Co., Ltd., fatty acid methyl ethoxylate
Porous inorganic powder: Examples 7 and 9 and Comparative Examples 3 and 5 are amorphous
Silica (Aerosil 300 (Japan Aerosil Co., Ltd.
)), Examples 8 and 10, and Comparative Examples 4 and 6 are crystalline silicic acid C.
a (Fluorite R (produced by Tokuyama Soda Co., Ltd., crystalline silicic acid
Lucium))

Further, the products prepared by adding 0.2 parts of the fragrance and 0.1 part of the enzyme to the compositions of Examples 7 to 10 were used and washed in an actual washing machine. I confirmed that I could wash it well.

[Brief description of drawings]

FIG. 1 is a flow sheet showing an example of the present invention.

─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. ⁶ Identification code Internal reference number FI technical display location C11D 17/06

Claims (2)

[Claims] 1. When a granular nonionic detergent composition is produced by stirring and granulating the following components (a) to (d) in the following amounts, (a) nonionic surfactant: 10 to 70 wt. % (B) Crystalline aluminosilicate: 5 to 50% by weight (c) Porous inorganic oxide powder: 0.2% by weight or more and less than 5% by weight (d) Sodium carbonate: 1 to 75% by weight for granulation 1 to 90% (weight basis) of the amount of at least one of the above-mentioned components (b), (c) and (d) used.
Of the above-mentioned (b),
The components (c), (d) and (a) are added into the stirring granulator to start the stirring granulation, and after that, until the end of the stirring granulation treatment, the powder for additional addition described above. A method for producing a granular nonionic detergent composition, characterized in that the detergent granules are obtained by continuously, stirring, or granulating the ingredients in a batch, divided or continuous manner. 2. The following components (a) to (d) are used in the following amounts, respectively, to produce a granular nonionic detergent composition by stirring and granulating: (a) nonionic surfactant: 10 to 70% by weight. % (B) Crystalline aluminosilicate: 5 to 50% by weight (c) Porous inorganic oxide powder: 0.2% by weight or more and less than 5% by weight (d) Sodium carbonate: 1 to 75% by weight 5% of the porous inorganic oxide powder of component (c)
The nonionic surfactant of the component (a) is dispersed on the above (weight basis), the obtained dispersion, (b) the crystalline aluminosilicate, the remaining (c) the porous inorganic oxide powder and (d). A method for producing a granular nonionic detergent composition, which comprises granulating sodium carbonate with stirring to produce detergent particles.