JP4912826B2 - Method for producing anionic surfactant granules - Google Patents

Description

  The present invention relates to a method for producing an anionic surfactant granular material. More specifically, for example, the present invention relates to a method for producing an anionic surfactant granular material that can be suitably used for clothing detergents, kitchen detergents, toothpaste foaming agents, powder shampoos, polymerization emulsifiers, cement foaming agents, and the like.

  As a method for producing an anionic surfactant powder or granular material, a method of spray drying an aqueous alkyl sulfate slurry (Patent Document 1), forming a thin film of high-concentration slurry on the inner surface of the heat transfer wall, A method of concentrating and drying (Patent Documents 2 and 3), a method of granulating simultaneously with drying while adding an anionic surfactant paste to a powder raw material under reduced pressure (Patent Document 4), and the like are known.

  However, the method described in Patent Document 1 has a problem that a large-scale drying apparatus is required because it includes a spray drying process. Furthermore, the methods described in Patent Documents 2 and 3 also have a problem that a large-scale drying apparatus is required. In the method described in Patent Document 4, a large-scale drying apparatus is not necessary, but an anionic surfactant adheres in the dryer, resulting in a decrease in yield and is not economical.

  As an adhesion suppression measure in the production method by stirring granulation of the cleaning composition, a method of blending an adhesion inhibitor (Patent Document 5), a method of imparting impact force to the granulator (Patent Document 6), a Froude number, A method for adjusting the addition rate of the liquid raw material (Patent Document 7) is known.

  However, the method of Patent Document 5 has a drawback that the concentration of impurities in the product becomes high because an adhesion inhibitor is blended in the raw material. The method of Patent Document 6 is not possible with a device having a rotating shaft in the vertical direction, and further has the disadvantage that the granulator itself must be rotated, so that it must be a sufficiently small device. . The method of Patent Document 7 is a manufacturing method in which a liquid raw material is added and each particle is surface-treated with the liquid raw material. When the liquid raw material is not continuously added, a technical solution has not been sufficiently achieved.

  As described above, the conventional technique for producing an anionic surfactant granular material has problems such as a large scale of the drying apparatus and adhesion of the anionic surfactant in the dryer. Restrictions remain, such as those in which the structure is limited and those in which liquid raw materials are added.

Therefore, there is a demand for a method for producing a high-quality anionic surfactant powder and a high-quality anionic surfactant granular material in which the scale of the drying apparatus is small and the anionic surfactant does not adhere to the dryer.
JP 54-106428 A JP-A-2-222498 Japanese Patent Laid-Open No. 5-331496 JP 2005-68413 A JP-A-7-133498 JP 2001-246238 A JP 2006-143998 A

  An object of the present invention is to provide a method of efficiently producing an anionic surfactant granular material with a small scale of a drying apparatus and less adhesion of an anionic surfactant to the inside of the drying apparatus.

  The present invention relates to a method for producing an anionic surfactant granule, which obtains an anionic surfactant granule while introducing gas along a granulator having a stirring blade or a wall surface in a dryer under reduced pressure.

  By the method of this invention, it can suppress that an anionic surfactant granular material adheres to the wall surface in a dryer or a granulator, and an anionic surfactant granular material with a high yield can be manufactured.

[Anionic surfactant]
The anionic surfactant used in the present invention is not particularly limited, and examples thereof include alkyl sulfates, polyoxyalkylene alkyl ether sulfates, α-olefin sulfates, alkylbenzene sulfonates, α-sulfo fatty acid ester salts and the like. . Of these, alkyl sulfates are preferred. Examples of the salt include alkali metal salts, alkaline earth metal salts, ammonium salts, alkanolamine salts and the like. Among these salts, alkali metal salts are preferable, and sodium salts, potassium salts, and mixtures of these salts are more preferable.

  Examples of the alkyl sulfate include alkyl sulfates represented by the formula (I).

(RO-SO ₃ ) _p M (I)
Wherein R is a linear or branched alkyl or alkenyl group having 8 to 24 carbon atoms, preferably 8 to 18 carbon atoms, M is an alkali metal atom, an alkaline earth metal atom, an alkanol-substituted or unsubstituted ammonium group. And the like, p is the valence of M and represents 1 or 2.)
The alkyl sulfate represented by the formula (I) is obtained by sulfating and further neutralizing a higher alcohol having 8 to 24 carbon atoms. In the sulfation reaction, unreacted substances may be present in the range of 10% by weight or less, preferably 5% by weight or less.

[Method for producing anionic surfactant powder]
In the method for producing an anionic surfactant granular material of the present invention, the pressure in the granulator or the dryer needs to be a reduced pressure from the viewpoint of suppressing the adhesion of the granular material, and is 0.5 to 50 kPa. 0.67 to 13.3 kPa is more preferable, and 2.0 to 8.0 kPa is particularly preferable from the viewpoint of the load on the vacuum pump and the airtightness of the granulator or dryer.

  The gas introduced into the granulator or dryer may be anything as long as it has no reactivity with the anionic surfactant, and examples thereof include air, inert gas, and water vapor. Examples of the inert gas include helium, nitrogen, argon, carbon dioxide gas, and the like. From the viewpoint of suppressing the load on the vacuum pump, a condensable gas is preferable, and water vapor is particularly preferable.

The larger the amount of gas introduced into the machine, the better from the viewpoint of suppressing adhesion of the granular material. However, from the viewpoint of the load of the vacuum pump, preferably inboard of the granular material 1kg per ^{0.5~10m 3 / h, 0.5~5.0m 3 /} h is more preferable. Here, the volume of gas is the volume at the temperature and pressure in the machine.

  The gas may be introduced along the wall surface in the machine, and can be introduced using a blowing nozzle or the like. The position, number, and shape of the blowing nozzle are not limited. However, it is better that the number of nozzles is larger because the gas flow introduced into the machine passes through the entire wall surface to suppress adhesion of powder particles. Further, the direction of the nozzle is particularly the circumferential direction among the directions along the wall surface, and the adhesion suppressing effect is enhanced by causing a swirling flow in the machine. Further, it is preferable to blow the gas in the same direction as the rotation direction of the stirring blade because a swirl flow is easily generated in the machine.

  The specific example of the granulator or dryer provided with the blowing nozzle used for this invention is shown to FIGS. FIG. 1 is a front view showing an example of an apparatus provided with one downward single tube 1 as a blowing nozzle. Gas is introduced from the single pipe 1 along the wall surface 2 in the machine. In FIG. 1, 3 is a stirring blade and 4 is a crushing blade. FIG. 2 is a plan view showing an example of an apparatus provided with two L-shaped tubes 5 and 5 ′ as blowing nozzles. Gas is introduced from the two L-shaped tubes 5 and 5 ′ along the circumferential direction of the wall surface 2 in the machine. At this time, it is preferable to introduce a gas in the same direction as the rotation direction of the stirring blade because a swirl flow can be created in the machine. FIG. 3 is a front view showing an example of an apparatus provided with a ring sparger 6 as a blowing nozzle, and FIG. 4 is a plan view thereof. The ring sparger has a plurality of holes, and a gas is introduced through the holes, and a curtain of airflow can be made along the wall surface 2 in the machine. Among these blowing nozzles, the L-shaped tube shown in FIG. 2 and the ring sparger shown in FIGS. 3 and 4 are preferable.

  The granulator or dryer used in the present invention is not particularly limited as long as it has a configuration having a stirring blade, but preferably has a crushing blade. Examples of the apparatus preferably used include, for example, Henschel mixer [manufactured by Mitsui Miike Chemical Co., Ltd.], high speed mixer [manufactured by Fukae Powtech Co., Ltd.], vertical granulator [manufactured by Pou Lec Co., Ltd.], Redige mixer [Matsuzaka Giken Co., Ltd.], Pro-Share Mixer [Pacific Kiko Co., Ltd.] and the like.

  In the present invention, it is preferable to control the temperature of the anionic surfactant powder in the machine so as to be in the range of preferably 50 to 150 ° C, more preferably 60 to 120 ° C. As a method for controlling the temperature in this manner, (1) the fluid number of the stirring blade, (2) the temperature of the jacket, (3) the method of appropriately adjusting the temperature of the gas introduced into the machine, and the like can be mentioned. Hereinafter, each method will be described in detail.

(1) Fluid number of stirring blade In this invention, it is preferable that the fluid number of the stirring blade represented by Formula (II) is 0.3-5.0, More preferably, it is 0.9-2.3. It is.

Fr = V / (R × g) ^0.5 (II)
(In the formula, Fr is the Froude number, V is the peripheral speed [m / s] of the tip of the stirring blade, R is the rotation radius [m] of the stirring blade, and g is the acceleration of gravity [m / s ² ].)
When the Froude number is 5.0 or less, the amount of powder rolling up in the machine and the centrifugal force can be suppressed, and the adhesion amount of the granular material can be reduced. Moreover, when it is 0.3 or more, the granular material is preferably sufficiently stirred. Moreover, since the frictional heat between the powder particles increases and the temperature increases as the fluid number increases, the temperature of the powder particles can be controlled by adjusting the fluid number.

(2) Jacket temperature The granulator or dryer used in the present invention is preferably provided with a jacket for adjusting the temperature of the granular material in the machine. Examples of the heating source include steam, warm water, and electric tracing, but warm water is preferable. The jacket temperature is preferably 115 ° C. or lower, and more preferably 100 ° C. or lower from the viewpoint of application to heat sensitive raw materials.

(3) Temperature of gas introduced into the machine The temperature of the gas introduced into the machine is not particularly limited. However, for example, when saturated water vapor is introduced, it is preferably 170 ° C. (0.8 MPa) or less, more preferably 150 ° C. (0.5 MPa) or less from the viewpoint of application to heat-sensitive raw materials.

Example 1
As a blowing nozzle, a vacuum dryer having a volume of 2500 L (FMD-1200JE, manufactured by Fukae Powtech Co., Ltd.) having one single downward pipe 1 having an inner diameter of 25 mmφ shown in FIG. 1 and having a stirring blade 3 and a crushing blade 4 is used. 543 kg of a powder of sodium alkylsulfate (Emal 10P-HD, manufactured by Kao Corporation, a mixture of 67 mol% of alkyl group, 28 mol% of carbon number 14 and 5 mol% of carbon number 16) , Pressure 5.3 kPa, jacket temperature 80 ° C., stirring blade rotation speed 55 rpm, stirring blade fluid number 1.8, crushing blade rotation speed 2000 rpm, steam blowing rate from single tube 1 60 kg / h (powder particles) 3.7m per 1kg ³ / h), and the condition 5 hours while blowing along the steam cabin wall 2 in the steam pressure 0.79 MPa, sodium alkyl sulfate It was prepared granular material of unsalted. As a result, the temperature of the granular material was 106.5 ° C., and the recovery rate was 86.2%.

Example 2
As a blowing nozzle, a vacuum dryer having a volume of 2500 L having two L-shaped tubes 5 and 5 ′ having an inner diameter of 25 mmφ shown in FIG. 2 and having a stirring blade and a crushing blade [FMD-1200JE type, manufactured by Fukae Powtech Co., Ltd.] 543 kg of alkyl sulfate sodium salt (Emal 10P-HD) powder was put in, pressure 5.3 kPa, jacket temperature 80 ° C., stirring blade rotation speed 55 rpm, stirring blade fluid number 1.8, and crushing blade rotation speed 2000 rpm. , Steam was blown from the L-shaped pipes 5 and 5 ′ at a rate of 60 kg / h of steam (3.6 m ³ / h per 1 kg of granular material) and steam pressure of 0.79 MPa along the wall surface 2 of the machine. It processed for 4 hours, blowing in the same direction as a rotation direction, and manufactured the granular material of the alkyl sulfate sodium salt. As a result, the granule temperature was 96.2 ° C. and the recovery rate was 94.9%.

Example 3
As a blowing nozzle, a vacuum dryer having a volume of 2500 L having a ring sparger 6 having an inner diameter of 10 mmφ and a number of holes of 16 shown in FIGS. Mold] was charged with 543 kg of powder of sodium alkyl sulfate (Emal 20P-2, manufactured by Kao Corporation, alkyl group 12 carbon atoms) with pressure inside the machine, pressure 5.3 kPa, jacket temperature 80 ° C., stirring blade rotation speed 55 rpm, stirring blade fluid number 1.8, crushing blade rotation speed 2000 rpm, steam blowing rate from ring sparger 6 20 kg / h (1.2 m ³ / h per 1 kg of granular material), Processed for 5 hours while blowing steam along the wall surface 2 in the machine under the condition of steam pressure of 0.29 MPa, and sodium alkyl sulfate salt powder It was prepared. As a result, the particle temperature was 98.6 ° C. and the recovery rate was 100%.

Example 4
The same alkyl sulfate sodium salt powder as in Example 1 in a 2500 L vacuum dryer [FMD-1200JE type, manufactured by Fukae Powtech Co., Ltd.] having the same volume as Example 2 having two L-shaped tubes, stirring blades and crushing blades 543 kg, pressure of 5.3 kPa, jacket temperature of 80 ° C., stirring blade rotation speed of 55 rpm, stirring blade fluid number of 1.8, crushing blade rotation speed of 2000 rpm, steam blowing rate of 20 kg / h (1 kg / kg of granular material) 2m ³ / h), steam was blown along the wall of the machine in the same direction as the rotation direction of the stirring blade for 3 hours under the conditions of a steam pressure of 0.79 MPa to produce sodium alkyl sulfate sodium salt granules did. As a result, the granule temperature was 96.0 ° C., and the recovery rate was 83.2%.

Example 5
The same alkyl sulfate sodium salt powder as in Example 3 in a vacuum dryer (Fukae Pautech Co., Ltd., FMD-1200JE type) having the same volume as Example 2 having two L-shaped tubes, stirring blades and crushing blades 543 kg, pressure 5.3 kPa, jacket temperature 80 ° C., stirring blade rotation speed 55 rpm, stirring blade fluid number 1.8, crushing blade rotation speed 2000 rpm, steam blowing rate 40 kg / h (2 per 1 kg of granular material) 4m ³ / h), steam was blown along the wall of the machine in the same direction as the rotation direction of the stirring blade for 4 hours under the conditions of a steam pressure of 0.29 MPa to produce sodium alkyl sulfate sodium salt granules did. As a result, the particle temperature was 90.7 ° C. and the recovery rate was 87.2%.

Example 6
The same alkyl sulfate sodium salt powder as in Example 3 in a vacuum dryer (Fukae Pautech Co., Ltd., FMD-1200JE type) having the same volume as Example 2 having two L-shaped tubes, stirring blades and crushing blades 543 kg of pressure, pressure 5.3 kPa, jacket temperature 80 ° C., stirring blade rotation speed 55 rpm, stirring blade fluid number 1.8, crushing blade rotation speed 2000 rpm, steam blowing rate 60 kg / h (3 per kg of granular material) 5m ³ / h), steam is blown along the wall of the machine in the same direction as the direction of rotation of the stirring blade for 4 hours under the conditions of a steam pressure of 0.79 MPa to produce sodium alkyl sulfate sodium salt granules did. As a result, the granule temperature was 92.9 ° C., and the recovery rate was 88.7%.

Example 7
The same alkyl sulfate sodium salt powder as in Example 1 in a 2500 L vacuum dryer [FMD-1200JE type, manufactured by Fukae Powtech Co., Ltd.] having the same volume as Example 2 having two L-shaped tubes, stirring blades and crushing blades 543 kg, pressure 5.3 kPa, jacket temperature 80 ° C., stirring blade rotation speed 40 rpm, stirring blade fluid number 1.3, crushing blade rotation speed 2000 rpm, steam blowing rate 60 kg / h (3 per kg of granular material) .6 m ³ / h), and steam pressure 0.79 MPa, steam is blown along the wall of the machine in the same direction as the direction of rotation of the stirring blade for 4.5 hours to obtain sodium alkyl sulfate salt granules Manufactured. As a result, the particle temperature was 99.2 ° C. and the recovery rate was 92.5%.

Comparative Example 1
Into a 2500 L vacuum dryer (Fukae Pautech Co., Ltd., FMD-1200JE type) having a stirring blade and a crushing blade, 543 kg of the same alkyl sulfate sodium salt powder as in Example 3 was placed, pressure 5.3 kPa, jacket temperature Processed for 10 hours without blowing gas under the conditions of 65 ° C., stirring blade rotation speed 55 rpm, stirring blade fluid number 1.8, and crushing blade rotation speed 2000 rpm. Manufactured. As a result, the particle temperature was 107.8 ° C. and the recovery rate was 63.7%.

Comparative Example 2
Into a 2500 L vacuum dryer (Fukae Pautech Co., Ltd., FMD-1200JE type) having a stirring blade and a crushing blade, 543 kg of the same alkyl sulfate sodium salt powder as in Example 1 was put, pressure 5.3 kPa, jacket temperature Sodium alkylsulfate powder granules treated at 80 ° C. under conditions of stirring blade rotation speed of 55 rpm, stirring blade fluid number of 1.8, and crushing blade rotation speed of 2000 rpm without blowing gas. Manufactured. As a result, the granule temperature was 109.5 ° C., and the recovery rate was 71.7%.

  Table 1 shows the production conditions and results of Examples 1 to 8 and Comparative Examples 1 and 2.

It is a front view which shows an example of the apparatus provided with the downward single pipe as a blowing nozzle. It is a top view which shows an example of the apparatus provided with two L-shaped pipes as a blowing nozzle. It is a front view which shows an example of the apparatus provided with the ring sparger as a blowing nozzle. FIG. 4 is a plan view of the apparatus of FIG. 3.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Single pipe 2 Wall surface 3 Stirring blade 4 Crushing blade 5, 5 'L-shaped pipe 6 Ring sparger

Claims (7)

After placing a powder of anionic surfactant dryer having a granulation function having a stirring blade, under reduced pressure, introducing a gas along the dryer wall having a granulation function having a stirring blade A method for producing an anionic surfactant granular material, wherein the anionic surfactant granular material is obtained.   The manufacturing method of the anionic surfactant granular material of Claim 1 which introduce | transduces gas in the same direction as the rotation direction of a stirring blade. The method for producing an anionic surfactant granular material according to claim 1 or 2, wherein the amount of gas introduced is 0.5 to 10 m ³ / h per 1 kg of the granular material in the machine. Anionic surfactant is an alkyl sulfate, a manufacturing method of the anionic surfactant powder according to any one of claims 1 to 3. Gas is a gas having no reactivity with the anionic surfactant, the production method of the anionic surfactant powder according to any one of claims 1 to 4. Cabin pressure is 0.5 to 50 kPa, the manufacturing method of the anionic surfactant powder according to any one of claims 1 to 5. Dryer with a further crushing blade having a granulation function having a stirring blade, a manufacturing method of the anionic surfactant powder according to any one of claims 1 to 6.

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