JP4108188B2 - Continuous production method of granular nonionic detergent composition - Google Patents

Description

【００３０】
【表２】

【００３１】
表１及び表２の結果から、ノニオン界面活性剤の添加時間が短すぎても、また逆に長すぎても、造粒機の付着が増加することがわかる。ノニオン界面活性剤の添加速度が長すぎた場合に、付着が増加する原因は明らかでないが、造粒速度とノニオン界面活性剤の供給速度とのバランスが関係しているものと思われる。
【００３２】
表１及び表２から、本発明の方法によれば、造粒機内部の付着量を抑制し、且つバッチ当たりの生産量を増加させることができる上に、粒度分布の狭い造粒物を得ることができることがわかる。更に、表２の実施例１０の結果から、２段階造粒により造粒物の粒度分布を広げることなしにバッチ当たりの生産量を増加させることができることがわかる。
【００３３】
【発明の効果】
請求項１の粒状ノニオン洗剤組成物の製造方法によれば、前記構成としたことから、造粒機内部の付着を抑制し、バッチ当たりの生産量を増加させることができる。
【００３４】
請求項２の粒状ノニオン洗剤組成物の製造方法によれば、撹拌造粒を２段階で実施したことから、粒度分布を広げることなしに更にバッチ当たりの生産量を増加させることができるという効果が加わる。[0001]
BACKGROUND OF THE INVENTION
TECHNICAL FIELD The present invention relates to a method for producing a granular nonionic detergent composition, and more specifically, a granular nonionic detergent composition capable of suppressing adhesion inside the agitation granulator and increasing the production amount per batch in the agitation granulation of the nonionic detergent. The present invention relates to a method for manufacturing a product.
[0002]
[Prior art]
Nonionic surfactants generally have low foaming properties, and their detergency is not easily affected by the hardness of water, and in particular, they are excellent in dirt and dirt dispersibility at low temperatures. Furthermore, it is an excellent surfactant with good biodegradability, low environmental impact, low toxicity and no safety problems. However, many nonionic surfactants are liquid at room temperature, and the non-ionic surfactants are not good because they are poorly mixed with cleaning builders and other powdered materials that are mixed during the production of granular nonionic detergent compositions. When the granular nonionic detergent composition as the main active agent is produced by stirring granulation, adhesion inside the apparatus is likely to occur, causing the fluidity and caking resistance of the granulated product to deteriorate, making stable continuous production difficult. There is a drawback. Moreover, since the change in bulk density between the start and end of granulation is large, only about 20-30 vol% of the granulator capacity can be produced, and the production amount per batch is further influenced by the above-mentioned deposits. Is not stable.
[0003]
Therefore, in JP-A-5-209200 and JP-A-5-125400, in order to obtain a granular nonionic detergent composition having a high bulk density and excellent fluidity and caking resistance, a mixing step-stir granulation step -In the process which consists of a fine powder coating process, the granulation method is proposed in which the adhesion layer of the detergent raw material is formed on the inner wall of the stirring type mixer in the stirring granulation process. However, it is not preferable that the adhesion layer grows with time and is repeatedly scraped off by the stirring blade because the load on the granulator may become unstable and the quality may become uneven.
[0004]
[Problems to be solved by the invention]
Accordingly, an object of the present invention is to provide a production method capable of suppressing adhesion inside the agitation granulator and increasing the production amount per batch when producing a granular nonionic detergent composition by agitation granulation. There is to do.
[0005]
[Means for Solving the Problems]
As a result of intensive research, the present inventors have achieved the above object by supplying a nonionic surfactant at a specific addition rate into a fluid powder raw material in a stirring granulator in stirring granulation. In addition, the inventors have found that the production amount can be increased without expanding the particle size distribution of the granulated product by carrying out stirring granulation in two stages, and the present invention has been achieved.
[0006]
That is, according to the present invention, first, when producing a granular nonionic detergent composition having a nonionic surfactant as a main active agent by stirring granulation,
B) First, the powder raw material is fluidized in the granulator by the rotation of the stirring blade,
B) Subsequently, a nonionic surfactant is supplied into the granulator at an addition rate satisfying the following formula (I).
A method for producing a granular nonionic detergent composition is provided.
Q / (N · D ³ ) = (1.0 to 9.0) × 10 ⁻⁵ (I)
[In formula, Q, N, and D represent the following respectively.
Q: Rate of addition of nonionic surfactant (m ³ / s)
N: Number of rotations of the stirring blade (1 / s)
D: Diameter of stirring blade (m)]
Second, when producing a granular nonionic detergent composition having a nonionic surfactant as a main active agent by stirring granulation,
C) First, some powder raw materials are fluidized in the granulator by the rotation of the stirring blades.
D) Subsequently, a part of the nonionic surfactant is granulated by supplying it into the granulator at the addition rate described in the above first-b) to prepare a first granulated product,
E) When the particle size of the first granulated product reaches a particle size range of 20 to 60% of the intended granulated product, the remaining powder raw material and the addition rate described in the above first-b) The remaining nonionic surfactant is supplied into the granulator to perform the second granulation.
A method for producing a granular nonionic detergent composition is provided.
[0007]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the present invention will be specifically described in detail.
In the method of the present invention, various nonionic surfactants can be used as the nonionic surfactant. Examples of preferable nonionic surfactants include the following.
[0008]
(1) Polyoxyalkylene alkyl (or alkenyl) obtained by adding an average of 3 to 30 moles, preferably 5 to 20 moles of an alkylene oxide having 2 to 4 carbon atoms to an aliphatic alcohol having 6 to 22 carbon atoms, preferably 8 to 18 carbon atoms ether. Among these, polyoxyethylene alkyl (or alkenyl) ether and polyoxyethylene polyoxypropylene alkyl (or alkenyl) ether are preferable.
(2) Polyoxyethyl alkyl (or alkenyl) phenyl ether.
[0009]
(3) A fatty acid alkyl ester alkoxylate represented by the following formula in which an alkylene oxide is added between ester bonds of a long-chain fatty acid alkyl ester.
R ¹ CO (OA) n OR ²
(R ¹ CO represents a fatty acid residue having 6 to 22 carbon atoms, preferably 8 to 18 carbon atoms. OA is an addition unit of alkylene oxide having 2 to 4 carbon atoms, preferably 2 to 3 carbon atoms such as ethylene oxide and propylene oxide. N represents the average number of moles of alkylene oxide added and is generally a number of 3 to 30, preferably 5 to 20. R ² is a lower group which may have a substituent of 1 to 3 carbon atoms. Represents an alkyl group.)
[0010]
(4) Polyoxyethylene sorbitan fatty acid ester.
(5) Polyoxyethylene sorbite fatty acid ester.
(6) Polyoxyethylene fatty acid ester.
(7) Polyoxyethylene hydrogenated castor oil.
(8) Glycerin fatty acid ester.
[0011]
Among the above nonionic surfactants, polyoxyethylene alkyl (or alkenyl) ether having a melting point of 40 ° C. or less and an HLB of 9 to 16 and fatty acid methyl ester ethoxylate obtained by adding ethylene oxide to fatty acid methyl ester are particularly preferably used. . These nonionic surfactants may be used as a mixture.
[0012]
The nonionic surfactant is generally contained in the granular nonionic detergent composition in an amount of 10 to 40% by weight, more preferably 12 to 35% by weight, and particularly preferably 15 to 30% by weight. If this amount is less than 10% by weight, the concentration of the nonionic surfactant in the resulting detergent particles is low and the bulk density is low. Therefore, a good cleaning effect cannot be obtained unless the amount of detergent used is increased. As a result, the result is contrary to downsizing, which is not preferable, and it is not preferable in terms of resource saving. On the other hand, if it exceeds 40% by weight, there is no particular problem in the case of batch production, but the amount of adhesion in the granulator increases during continuous production, making it difficult to produce stably. It is not preferable.
[0013]
In the method of the present invention, as a powder raw material, a builder or other powder raw material usually used in a detergent is used. For example, zeolite, tripolyphosphate, citrate, succinate, polyacrylate, acrylic acid-maleic acid copolymer, chelate builder such as EDTA, alkali metal carbonate (sodium carbonate, potassium carbonate, etc.), Alkali builders such as alkali metal silicates (sodium silicate, potassium silicate, etc.), layered polysilicates (macatite, kanemite, etc.) are included. In addition, powders such as mirabilite, silica, calcium carbonate, starch, and metal soap can be used.
[0014]
Nonionic surfactant and stirring granulation in such an amount that the powder raw material is generally mixed in a granular nonionic detergent composition in an amount of 40 to 80% by weight, preferably 40 to 75% by weight, more preferably 50 to 70% by weight. Is done. When the blending amount of the powder raw material is less than 40% by weight, the fluidity is lowered.
[0015]
In the method of the present invention, as described above, first, the powder raw material is fluidized in the granulator by the rotation of the stirring blade, and then the nonionic surfactant is granulated at an addition rate satisfying the following formula (I). Supplied on board.
Q / (N · D ³ ) = (1.0 to 9.0) × 10 ⁻⁵ (I)
However, in the formula, Q: addition rate of nonionic surfactant (m ³ / s)
N: Number of rotations of stirring blade (l / s)
D: Diameter of stirring blade (m)
Represents.
[0016]
That is, the nonionic surfactant is adjusted so that the value of Q / (N · D ³ ) (hereinafter sometimes referred to as an addition index) is in the range of (1.0 to 9.0) × 10 ^−5. Is supplied into the fluidized powder raw material, the adhesion of the detergent raw material to the inner wall of the granulator can be suppressed, and the production amount per batch can be increased. The value of the added index is preferably in the (2.0~8.0) × 10 ^-5, it is further preferable that the (3.0~7.0) × 10 ^-5. If the value of the addition index is less than 1.0 × 10 ⁻⁵ , the adhesion to the apparatus increases, the production volume varies between batches, and the particle size distribution becomes broad, and conversely 9.0 × Even if it exceeds 10 ⁻⁵ , the adhesion of the apparatus increases and the problem arises that the production volume between batches varies.
In Example 1 of the above-mentioned JP-A-5-209200, Q / (N · D ³ ) = 9.7 × 10 ⁻⁵ , and in Example 1 of JP-A-5-125400, Q / (N · D ³ ) = 2.4 × 10 ⁻⁴ .
[0017]
Further, in the method of the present invention, it is very preferable to carry out stirring granulation in two stages because the production amount can be increased without widening the particle size distribution of the granulated product.
That is, in the second method of the present invention, a part of the powder raw material is first fluidized in the granulator by the rotation of the stirring blade, and then a part of the nonionic surfactant is converted to the general formula (I). Is supplied into the granulator at an addition rate satisfying the above. The particle size of the produced granulated product is 20 to 60%, preferably 30 to 50% of the intended granulated product (second granulated product) (the average particle size of the second granulated product is When the average particle size is 500 μm, granulation is performed until the average particle size becomes 100 to 300 μm, preferably 150 to 250 μm, to obtain a first granulated product.
When the particle size of the granulated product falls within the above range, the remaining powder raw material is supplied into the granulator, and the remaining nonionic surfactant is granulated at an addition rate satisfying the general formula (I). The product is supplied into the machine and second granulation is performed to obtain a target second granulated product. The amount of the powder raw material and the nonionic surfactant supplied to the granulator in the second granulation is usually 30 to 70% by weight, preferably 40 to 60% by weight of the first granulation.
[0018]
As the granulator used in the method of the present invention, any type of agitation granulator capable of mixing and agglomerating the powder raw material and the nonionic surfactant can be used. A stirring granulator having a shaft, equipped with a stirring blade for overall mixing and a stirring blade for crushing, and having a clearance of 30 mm or less between the stirring blade and the inner wall surface of the granulator is preferable. Further, those equipped with a serrated stirring blade, such as a Laedige mixer (manufactured by Matsubo Co., Ltd.), a proshear mixer (manufactured by Taiyo Kiko Co., Ltd.), etc. are particularly preferred.
[0019]
The temperature of stirring granulation is generally 20 to 60 ° C, preferably 30 to 50 ° C, more preferably 35 to 50 ° C. When the temperature is lower than 20 ° C., granulation is difficult to proceed, which is not preferable. On the other hand, if the temperature is higher than 60 ° C., it is not preferable because adhesion to the granulator tends to occur.
[0020]
In the method of the present invention, an oil-absorbing carrier and a nonionic gelling agent blended to prevent exudation of nonion under high temperature and high humidity and to improve the fluidity and caking resistance of detergent particles are added to the powder raw material. Is highly preferred. The preferred oil-absorbing carrier is an oil-absorbing amount represented by JIS-K6220 test method of 80 ml / 100 g or more, preferably 150 to 600 ml / 100 g, and a bulk density of 0.1 g / cc, preferably Is preferably used in the range of 0.001 to 0.08 g / cc. Examples of such an oil-absorbing carrier include amorphous silicic acid, amorphous calcium silicate, amorphous aluminosilicate, magnesium silicate, magnesium carbonate, calcium carbonate, spinel, mullite, cordierite, and starch decomposition products. These can also be used as a mixture.
[0021]
Examples of preferred nonionic gelling agents include 12-hydroxystearic acid, dibenzylidene sorbitol, lithium stearate, aluminum palmitate, lithium 2-ethylhexanoate, 12-hydroxyaluminum stearate, lauroylglutamic acid dibutylamide, lauroylglutamic acid. Stearylamide, dicaproyl lysine lauryl amide, dicaproyl lysine lauryl ester, lauroyl phenylalanine lauryl amide, polystyrene polybutadiene block copolymer, polyacrylamide-isoparaffin mixture, block copolymer of polystyrene block and polybutadiene block, dextrin palmitate, etc., or These mixtures are mentioned.
[0022]
In the method of the present invention, in the granular nonionic detergent composition, clay minerals and minor components normally incorporated in the detergent, such as fluorescent agents, enzymes, bleaching agents, antistatic agents, surface modifiers, anionic surfactants, Anti-contamination agents, extenders, fragrances, reducing agents, etc. can be blended, but these components may be blended in the mixing process or in the detergent particles obtained in the granulation process. Good.
[0023]
The following are shown as specific examples of components blended in other detergents.
(1) Clay mineral:
Montmorillonite, nontronite, beidellite, pyrophyllite, saponite, hectorite, stevensite, talc, etc.
(2) Fluorescent agent:
Bis (triazinylamino) stilbene disulfonic acid derivative, bis (sulfostyryl) biphenyl salt [Tinopearl CBS] and the like.
(3) Enzyme:
Lipase, protease, cellulase, amylase, etc.
(4) Bleach:
Percarbonate, perborate, etc.
(5) Antistatic agent:
Cationic surfactants such as dialkyl quaternary ammonium salts.
(6) Surface modifier:
Fine calcium carbonate, fine zeolite, polyethylene glycol, etc.
(7) Anionic surfactant:
α-sulfo fatty acid methyl ester salt, linear alkylbenzene sulfonate, α-olefin sulfonate, alkyl sulfate ester salt, fatty acid soap and the like.
(8) Recontamination inhibitor:
Cellulose derivatives such as carboxymethylcellulose.
(9) Bulking agent:
Sodium sulfate, potassium sulfate, sodium hydrochloride and the like.
(10) Fragrance:
(11) Reducing agent:
Sodium sulfite, potassium sulfite and the like.
[0024]
Furthermore, the detergent particles produced as described above may be coated by adding a coating agent in a rolling drum, for example. Thereby, a flow characteristic can be improved. As the coating agent, an inorganic powder having a JIS 200 mesh sieve passing rate of 50% or more is suitable. Examples of the material include carbonates such as sodium carbonate and calcium carbonate, amorphous silica, calcium silicate, and silicic acid. Silicates such as magnesium and aluminosilicates such as zeolite can be used. The coating agent is generally used in the granular nonionic detergent composition of the present invention in an amount of 0.5 to 15% by weight, preferably 1 to 10% by weight.
[0025]
【Example】
Hereinafter, the present invention will be described in more detail with reference to examples and comparative examples.
[0026]
<Raw materials>
In addition, the nonionic surfactant, powder raw material, and coating agent which were used by the Example and the comparative example are as follows.
Nonionic surfactant C ₁₂ H ₂₅ O (CH ₂ CH ₂ O) ₆ H (water content 6%)
Powder raw material (1) Powder raw material A
P-type zeolite: Crossfield (2) Powder raw material B
Sodium carbonate: Asahi Glass Co., Ltd., light ash (3) Powder raw material C
Sodium carbonate: manufactured by Asahi Glass Co., Ltd., granular ash coating agent P-type zeolite: manufactured by Crossfield Co., Ltd.
Examples 1-9 and Comparative Examples 1-2
Various powder raw materials in the amounts shown in Table 1 (Examples) and Table 2 (Comparative Examples) were put into a Raydege mixer [M-20 type manufactured by Matsubo Co., Ltd., internal volume 20 L, stirring blade diameter 0.3 m]. For 30 seconds. Subsequently, the nonionic surfactant was supplied at the speed shown in Tables 1 and 2, and granulated to about 500 μm. Finally, the coating agent in the amount shown in Table 1 and Table 2 was added and mixed for 30 seconds to obtain a granular nonionic detergent composition (Examples 1 to 5 were obtained by adding the nonion while keeping the number of revolutions of the granulator constant. Is a time change). The evaluation result of the obtained granular nonionic detergent composition is shown in Table 1 (Example) and Table 2 (Comparative Example).
[0028]
Example 10
Various powder raw materials in the amounts shown in Table 2 were put into a Laedige mixer [M-20 type manufactured by Matsubo Co., Ltd., internal volume 20 L, stirring blade diameter 0.3 m] and mixed for 30 seconds. Next, the nonionic surfactant is supplied at the rate shown in Table 2, and when the granulated product reaches 150 to 200 μm after the completion of the supply, the powder raw material and the nonionic surfactant are added in the same manner, and finally to about 500 μm. Granulated. Finally, the coating agent in the amount shown in Table 2 was added and mixed for 30 seconds to obtain a granular nonionic detergent composition. The evaluation results of the obtained granular nonionic detergent composition are shown in Table 2.
[0029]
[Table 1]

[0030]
[Table 2]

[0031]
From the results of Tables 1 and 2, it can be seen that the adhesion of the granulator increases even if the addition time of the nonionic surfactant is too short and conversely too long. The reason why the adhesion increases when the addition rate of the nonionic surfactant is too long is not clear, but it seems that the balance between the granulation rate and the supply rate of the nonionic surfactant is related.
[0032]
From Table 1 and Table 2, according to the method of the present invention, the amount of adhesion inside the granulator can be suppressed, the production amount per batch can be increased, and a granulated product having a narrow particle size distribution can be obtained. You can see that Furthermore, it can be seen from the results of Example 10 in Table 2 that the production amount per batch can be increased without widening the particle size distribution of the granulated product by two-stage granulation.
[0033]
【The invention's effect】
According to the manufacturing method of the granular nonionic detergent composition of Claim 1, since it was set as the said structure, adhesion inside a granulator can be suppressed and the production amount per batch can be increased.
[0034]
According to the method for producing a granular nonionic detergent composition according to claim 2, since the stirring granulation is carried out in two stages, there is an effect that the production amount per batch can be further increased without widening the particle size distribution. Join.

Claims (1)

In nonionic surfactant as a main active agent containing 15 to 30 wt%, the granular nonionic detergent compositions containing 40 to 80 wt% powder raw materials produced by stirring granulation,
C ) First, some powder raw materials are fluidized in the granulator by the rotation of the stirring blades.
D ) Subsequently, a part of the nonionic surfactant is granulated by supplying it into the granulator at an addition rate satisfying the following formula (I) to prepare a first granulated product,
E) When the particle size of the first granulated product reaches an average particle size range of 20 to 60% of the average particle size of the intended granulated product, the remaining powder raw material and the following formula (I) The remaining nonionic surfactant is supplied into the granulator at an addition rate that satisfies the above conditions, the second granulation is performed, and the granulation operation is performed at a granulator internal temperature of 20 to 60 ° C. A method for producing a granular nonionic detergent composition.
Q / (N · D ³ ) = (1.0 to 9.0) × 10 ⁻⁵ (I)
[In formula, Q, N, and D represent the following, respectively.
Q: Rate of addition of nonionic surfactant (m ³ / s)
N: Number of rotations of the stirring blade (1 / s)
D: Diameter of stirring blade (m)]